CN104975199B - The preparation method by extrusion molding thereof of metal/reinforcement composite material in alternating magnetic field - Google Patents

The preparation method by extrusion molding thereof of metal/reinforcement composite material in alternating magnetic field Download PDF

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Publication number
CN104975199B
CN104975199B CN201510361545.XA CN201510361545A CN104975199B CN 104975199 B CN104975199 B CN 104975199B CN 201510361545 A CN201510361545 A CN 201510361545A CN 104975199 B CN104975199 B CN 104975199B
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magnetic field
alternating magnetic
extrusion molding
metal
pug
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CN104975199A (en
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李静
袁玮
彭晓领
杨艳婷
徐靖才
王攀峰
金红晓
金顶峰
洪波
王新庆
葛洪良
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China Jiliang University
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China Jiliang University
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Abstract

The invention discloses in magnetostatic field functionally gradient material (FGM) preparation method by extrusion molding thereof.Its step is:1)By ferromagnetic metal and the ceramic mixed-powder of weak magnetic, organic solvent, dispersant and binding agent are added, it is uniform to mix, obtain pug;2)Pug is carried out into extrusion molding in an extruder, extrusion pressure is 0.2~0.8MPa, apply magnetostatic field at extrusion, magnetic field intensity is 0.01~2T, and then obtains green compact;3)After the completion of 20~80 DEG C of dryings, it is sintered, is sintered in the environmental protection of argon or nitrogen, sintering temperature is 1200~1500 DEG C, is incubated 4h, then furnace cooling.This have the advantage that:Composition continuously varying gradient material can be prepared;Improve the formality simplification of production functionally gradient material (FGM), cost reduction, performance using ripe extruding-out process.

Description

The preparation method by extrusion molding thereof of metal/reinforcement composite material in alternating magnetic field
Technical field
The present invention relates in a kind of alternating magnetic field metal/reinforcement composite material preparation method by extrusion molding thereof, belong to material system Standby field.
Background technology
Extrusion molding refers to material by the effect between extruder barrel and screw rod, and thermoplastification is received on side, while by screw rod forward Push, continue through head and make a kind of processing method of various cross section articles or semi-products.Traditional extrusion molding application In the processing of thermoplastic and rubber, dispensing, pelletize, sizing material filtration etc. can be carried out, be can be continuously produced, manufacture various continuous Product such as tubing, section bar, sheet material (or sheet material), thin film, electric wire cladding, rubber tire tread bar, inner-tube cylinder, sealing strip Deng its production efficiency height.With the development of technology, extrusion molding is also used for the molding of ceramic material and prepares.
The diverse location consecutive variations of the composition referred to because of material of functionally gradient material (FGM), structure in material internal, so as to cause One class composite of performance continually varying.Main preparation methods have powder compacting, vapour deposition process, Self-propagating Reaction Synthesis, Plasma spraying, electrocasting, galvanoplastic, laser sintered and centrifugal casting etc..But these preparation methoies exist important Limitation.As powder compacting is difficult to material component continuous and even variation;Vapour deposition is difficult to obtain big thickness material;From climing Prolong burning consistency relatively low;There is the interface of composition mutation in each painting interlayer of plasma spraying;Etc..These methods require complicated Technique or equipment, lack the preparation method of simplicity, be major reason that limitation function functionally gradient material (FGM) further develops.Therefore, If ripe metal or ceramic forming material means, for preparing FGM, undoubtedly can be had great importance And vast potential for future development.
At present, for many important FGMs such as:ZrO2/Ni、ZrO2/ steel, Al2O3/ Ni, SiC/Fe etc., gold The category transition metal such as constituent element Fe, Ni, Co belongs to ferromagnetic material, and ceramic component A l2O3、ZrO2、SiC、 AlN、Si3N4Etc. being Weak magnetic substance.Ferromagnetic material has ferromagnetism below Curie temperature, and weak magnetic substance is insensitive to magnetic field.Using two The difference of magnetic property between person, our group developments prepare the skill of functionally gradient material (FGM) in magnetostatic field using extruding forming method Art.
Regrettably, although said method can prepare FGM, the magnetic property of sample constituent element is had will Ask.There must be ferromagnetism in the component of slurry(Ferromagnetism, ferrimagnetism)Constituent element and weak magnetic(It is anti-ferromagnetism, paramagnetism, diamagnetic Property)Constituent element, otherwise can not be prepared using said method.Therefore, there is significant limitations in said method.Our groups are original Update on experiment basis, and make a breakthrough.On the basis of extrusion molding, metal group is controlled using alternating magnetic field The movement of unit, has successfully prepared the continuous functionally gradient material (FGM) of composition.
The present invention principle be:Metal material generally has good electric conductivity, can be because of the company in magnetic field in alternating magnetic field Continuing change and faradic current being produced in material internal, judged according to Lenz's law, the magnetic field that induced current is produced should be obstruction The change of interior flux.Therefore, Induced magnetic field and alternating magnetic field can produce the effect of power, magnetic forceFSize be:
Wherein,VIt is particle volume,MFor granule induced magnetism intensity, gradHFor magnetic field gradient.Magnetization M and input Current intensity is directly related, and current intensity is bigger, then the intensity of magnetization of inducting is bigger.Magnetic field gradient is had with granule location Close:In coil center of inside position, Distribution of Magnetic Field is uniform, and magnetic field gradient is zero, therefore the magnetic force that granule is subject to is zero;In coil End position, magnetic field gradient are maximum, and at the position, the magnetic force that metallic particles is subject to is maximum.Therefore, metallic particles is subject to magnetic force Size and the position of current intensity, the frequency of alternating magnetic field and metal in magnetic field have relation.Polymer and ceramic material Generally resistivity is very high, does not have vortex and produces, therefore do not affected by alternating magnetic field in alternating magnetic field.Then, based on metal Different to alternating magnetic field with polymer, ceramic constituent element is corresponding, can control metal constituent element in compound system using alternating magnetic field Interior distribution, preparing metal by extrusion moulding strengthens gradient composites.
The outstanding advantages of this method are exactly to apply alternating magnetic field to prepare composite on the basis of extruding-out process, are led to The technological parameters such as adjustment current intensity, frequency are crossed, composition consecutive variations and controllable graded composite material can be easily prepared Material, cost are substantially reduced.
The content of the invention
It is an object of the invention to provide in a kind of alternating magnetic field metal/reinforcement composite material preparation method by extrusion molding thereof.
Its step of is:
1)It is prepared by pug
By the metal of good electric conductivity in pug mill(One kind in Cu, Al, Ag, Mg, Zn, Fe etc.)With high resistivity (ZrO2、Al2O3、SiO2、SiC、Si3N4、B4One kind in C etc.)Mixed-powder, adds organic solvent, dispersant and binding agent, It is uniform to mix, obtain pug.Organic solvent is the one kind in ethanol, butanone, butanone or trichloro ethylene, organic solvent volume point Number for slurry 20~60%;Dispersant is herring oil, phosphate ester, glycerol trioleate or triethanolamine, and dispersant is slurry body The 0.2~5% of fraction;Bonding agent is polyvinyl butyral resin or polyvinyl alcohol, bonding agent for stock quality fraction 10~ 30%;
2)Extrusion molding in alternating magnetic field
Pug is carried out into extrusion molding in an extruder, extrusion pressure is 0.2~0.8MPa, at extrusion applies alternation Magnetic field, sample are located at alternating magnetic field end turn, and current intensity is 0.1~20A, and power frequency is 102~105Hz, and then obtain Green compact;
By action of alternating magnetic field, the metal inside of electric conductivity produces induced current, and then produces Induced magnetic field, Induced magnetic field It is driven metal with the interaction between nascent magnetic field, and then the forming component gradient in system.Reduce alternating current Intensity and frequency, the driving force that metal constituent element is subject to are reduced, and component gradient reduces.Improve alternating current intensity and frequency, metal The driving force increase that constituent element is subject to, component gradient then increase.In the presence of alternating magnetic field, alternating current intensity and frequency are from little During increase, metal and ceramic particle are built up to two ends respectively;
3)It is dried and sintering
After the completion of 20~80 DEG C of dryings, it is sintered, is sintered in the environmental protection of argon or nitrogen, sintering temperature is 1200~1500 DEG C, 4h is incubated, then furnace cooling;
The sample Jing electron probing analysis of preparation, metal constituent element are distributed in continuous gradient inside system.
It is an advantage of the invention that:
1)By applying alternating magnetic field, the functionally gradient material (FGM) of various thickness can be prepared in the range of very big composition;
2)Change the parameters such as current intensity, frequency, the distribution gradient of component in material can be controlled;
3)Make to prepare the formality simplification of functionally gradient material (FGM), cost reduction using ripe technique extruding forming method.
Specific embodiment
Embodiment 1:
1)It is prepared by pug
By the Ni metal of good electric conductivity and the ZrO of high resistivity in pug mill2Mixed-powder, adds organic solvent second Alcohol, dispersant herring oil and binding agent vinyl butyral, it is uniform to mix, obtain pug.Organic solvent volume fraction is pug 20%, the volume fraction of dispersant is 0.2%, and the mass fraction of bonding agent is the 10% of pug;
2)Extrusion molding in alternating magnetic field
Pug is carried out into extrusion molding in an extruder, extrusion pressure is 0.2MPa, applies alternating magnetic field at extrusion, Sample is located at alternating magnetic field end turn, and current intensity is 0.1A, and power frequency is 102Hz, and then obtain green compact;
3)It is dried and sintering
After the completion of 20 DEG C of dryings, it is sintered, is sintered in the environmental protection of argon, sintering temperature is 1200 DEG C, is protected Warm 4h, then furnace cooling.
Embodiment 2:
1)It is prepared by pug
By the metal Al of the good electric conductivity and Al of high resistivity in pug mill2O3Mixed-powder, adds organic solvent first Ethyl ketone, dispersant phosphate ester and binding agent polyvinyl alcohol, it is uniform to mix, obtain pug.Organic solvent volume fraction is pug 30%, the volume fraction of dispersant is 1%, and the mass fraction of bonding agent is the 15% of pug;
2)Extrusion molding in alternating magnetic field
Pug is carried out into extrusion molding in an extruder, extrusion pressure is 0.4MPa, applies alternating magnetic field at extrusion, Sample is located at alternating magnetic field end turn, and current intensity is 0.5A, and power frequency is 103Hz, and then obtain green compact;
3)It is dried and sintering
After the completion of 30 DEG C of dryings, it is sintered, is sintered in the environmental protection of nitrogen, sintering temperature is 1300 DEG C, is protected Warm 4h, then furnace cooling.
Embodiment 3:
1)It is prepared by pug
By the metal Ag of the good electric conductivity and SiO of high resistivity in pug mill2Mixed-powder, adds organic solvent fourth Ketone, dispersant glycerol trioleate and binding agent vinyl butyral, it is uniform to mix, obtain pug.Organic solvent volume fraction For the 40% of pug, the volume fraction of dispersant is 2%, and the mass fraction of bonding agent is the 20% of pug;
2)Extrusion molding in alternating magnetic field
Pug is carried out into extrusion molding in an extruder, extrusion pressure is 0.5MPa, applies alternating magnetic field at extrusion, Sample is located at alternating magnetic field end turn, and current intensity is 1A, and power frequency is 104Hz, and then obtain green compact;
3)It is dried and sintering
After the completion of 40 DEG C of dryings, it is sintered, is sintered in the environmental protection of nitrogen, sintering temperature is 1400 DEG C, is protected Warm 4h, then furnace cooling.
Embodiment 4:
1)It is prepared by pug
By the metal Mg of good electric conductivity and the SiC mixed-powders of high resistivity in pug mill, organic solvent three is added Vinyl chloride, dispersant triethanolamine and binding agent polyvinyl alcohol, it is uniform to mix, obtain pug.Organic solvent volume fraction is mud The 50% of material, the volume fraction of dispersant is 3%, and the mass fraction of bonding agent is the 30% of pug;
2)Extrusion molding in alternating magnetic field
Pug is carried out into extrusion molding in an extruder, extrusion pressure is 0.6MPa, applies alternating magnetic field at extrusion, Sample is located at alternating magnetic field end turn, and current intensity is 5A, and power frequency is 105Hz, and then obtain green compact;
3)It is dried and sintering
After the completion of 60 DEG C of dryings, it is sintered, is sintered in the environmental protection of nitrogen, sintering temperature is 1450 DEG C, is protected Warm 4h, then furnace cooling.
Embodiment 5:
1)It is prepared by pug
By the metal Zn of the good electric conductivity and Si of high resistivity in pug mill3N4Mixed-powder, adds organic solvent second Alcohol, dispersant phosphate ester and binding agent polyvinyl alcohol, it is uniform to mix, obtain pug.Organic solvent volume fraction is pug 60%, the volume fraction of dispersant is 5%, and the mass fraction of bonding agent is the 18% of pug;
2)Extrusion molding in alternating magnetic field
Pug is carried out into extrusion molding in an extruder, extrusion pressure is 0.8MPa, applies alternating magnetic field at extrusion, Sample is located at alternating magnetic field end turn, and current intensity is 10A, and power frequency is 105Hz, and then obtain green compact;
3)It is dried and sintering
After the completion of 80 DEG C of dryings, it is sintered, is sintered in the environmental protection of nitrogen, sintering temperature is 1500 DEG C, is protected Warm 4h, then furnace cooling.
Embodiment 6:
1)It is prepared by pug
By the metal Fe of the good electric conductivity and B of high resistivity in pug mill4C mixed-powders, add organic solvent first Ethyl ketone, dispersant glycerol trioleate and binding agent vinyl butyral, it is uniform to mix, obtain pug.Organic solvent volume point Number for pug 50%, the volume fraction of dispersant is 0.8%, and the mass fraction of bonding agent is the 22% of pug;
2)Extrusion molding in alternating magnetic field
Pug is carried out into extrusion molding in an extruder, extrusion pressure is 0.2MPa, applies alternating magnetic field at extrusion, Sample is located at alternating magnetic field end turn, and current intensity is 20A, and power frequency is 104Hz, and then obtain green compact;
3)It is dried and sintering
After the completion of 70 DEG C of dryings, it is sintered, is sintered in the environmental protection of nitrogen, sintering temperature is 1500 DEG C, is protected Warm 4h, then furnace cooling.
In various embodiments above, prepared sample Jing electron probing analysis finds, in material internal metal constituent element is in Continuous gradient is distributed.

Claims (5)

1. in alternating magnetic field metal/reinforcement composite material preparation method by extrusion molding thereof, it is characterised in that it the step of be:
1)It is prepared by pug
By the metal of good electric conductivity and the mixed-powder of high resistivity material composition in pug mill, add organic solvent, divide Powder and binding agent, it is uniform to mix, obtain pug;
The metal of described good electric conductivity is the one kind in Cu, Al, Ag, Mg, Zn and Fe;
Described high resistivity material is ZrO2、Al2O3、SiO2、SiC、Si3N4And B4One kind in C;
2)Extrusion molding in alternating magnetic field
Pug is carried out into extrusion molding in an extruder, extrusion pressure is 0.2~0.8MPa, at extrusion applies alternation magnetic , sample is located at alternating magnetic field end turn, and current intensity is 0.1~20A, and power frequency is 102~105Hz, and then given birth to Base;
3)It is dried and sintering
After the completion of 20~80 DEG C of dryings, it is sintered, is sintered in the environmental protection of argon or nitrogen, sintering temperature is 1200 ~1500 DEG C, 4h is incubated, then furnace cooling.
2. in alternating magnetic field according to claim 1 metal/reinforcement composite material preparation method by extrusion molding thereof, its feature It is that described organic solvent is the one kind in ethanol, butanone, butanone or trichloro ethylene, organic solvent volume fraction is slurry 20~60%.
3. in alternating magnetic field according to claim 1 metal/reinforcement composite material preparation method by extrusion molding thereof, its feature It is that described dispersant is herring oil, phosphate ester, glycerol trioleate or triethanolamine, dispersant is slurry volume fraction 0.2~5%.
4. in alternating magnetic field according to claim 1 metal/reinforcement composite material preparation method by extrusion molding thereof, its feature It is that described binding agent is polyvinyl butyral resin or polyvinyl alcohol, binding agent for stock quality fraction 10~30%.
5. in alternating magnetic field according to claim 1 metal/reinforcement composite material preparation method by extrusion molding thereof, its feature Alternating magnetic field described in being is produced by coil by alternating current.
CN201510361545.XA 2015-06-28 2015-06-28 The preparation method by extrusion molding thereof of metal/reinforcement composite material in alternating magnetic field Expired - Fee Related CN104975199B (en)

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CN105499570B (en) * 2015-12-25 2017-08-22 吉林大学 A kind of 3D printing method of the cermet functionally gradient part in alternating magnetic field
CN105772727B (en) * 2016-04-11 2017-10-10 吉林大学 A kind of 3D printing forming method of metal material gradient parts

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CN1915625A (en) * 2006-09-01 2007-02-21 浙江大学 Method for preparing gradient material of strong magnetism and weak magnetism through pressure filtration molding in pulse magnetism
CN1915626A (en) * 2006-09-01 2007-02-21 浙江大学 Method for preparing gradient material of strong magnetism and weak magnetism through flow casting molding in pulse magnetism
CN1944018A (en) * 2006-09-01 2007-04-11 浙江大学 Method for preparing strong magnetic-weak magnetic gradient material formed by slip casting in pulse magnetic field
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CN101503299A (en) * 2009-02-06 2009-08-12 中国计量学院 Gel injection moulding preparation for gradient material in rotating magnetic field
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