CN1304195C - Micelle ceramic/metal block composite material and preparation method thereof - Google Patents
Micelle ceramic/metal block composite material and preparation method thereof Download PDFInfo
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- CN1304195C CN1304195C CNB2004100971967A CN200410097196A CN1304195C CN 1304195 C CN1304195 C CN 1304195C CN B2004100971967 A CNB2004100971967 A CN B2004100971967A CN 200410097196 A CN200410097196 A CN 200410097196A CN 1304195 C CN1304195 C CN 1304195C
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Abstract
The present invention discloses a ceramic / metal composite material with a novel structure and a preparing technology of the ceramic / metal composite material, which belongs to a preparing technology of composite materials. The ceramic / metal composite material is formed by that the combination of honeycomb sealed multiple-cellular ceramics and intracellular metal or alloy. The micelle ceramic / metal block composite material has the preparing process: selecting a plurality of micrometers to several tens of micrometers of the metal or the alloy and a plurality of nanometers to several tens of nanometers of the ceramic coating powder; mixing the metal or the alloy and the ceramic coating powder according to a certain volumetric proportion; uniformly coating a basic powder surface with the nanometer coating powder completely by a polishing method; cold compression, shaping, sintering, and pycnosis composite sinter moulding by modules. The composite material has the advantages of simple process, convenient operation and programmable control for a sintering process. The cellular ceramic / metal composite material which is prepared by adopting the technical scheme of the present invention has a specific composite mode which makes the composite material have the ceramic performance and the characteristics of a traditional metal composite material, and through the adjustment of components of raw materials, the structural composite material has ideal rationalization and composite mechanical properties.
Description
Technical field
The invention belongs to the Composite Preparation technology, particularly micelle ceramic/metallic composite of a kind of new structure and preparation method thereof.
Technical background
Ceramic/metal composite materials mainly contains ceramic reinforced metal-base composites and metal toughening ceramic based composites two big classes, these ceramic/metal composite materials are based on structural material design mostly, the research focus concentrates on the comprehensive mechanical performance of material, mainly be intensity and toughness, obtained prominent achievement.The preparation method mainly contains hot extrusion, die casting, infiltration, PVD, centrifugal casting, powder metallurgy and growth in situ etc., and adding or spontaneous hardening constituent mostly are discrete (particle, short fiber etc.) or stereo weaving netted (part long fibre) in the metallic matrix.The metal ceramic gradient functional material causes the many material scholars' in the world concern recently, and the research of relevant FGM has obtained bigger progress.Distinguishing features such as discharge plasma sintering is a kind of brand-new PM technique, and it has, and programming rate is fast, sintering time is short can be used to prepare metal material, ceramic material, also can be used to prepare nano bulk material, function-graded material etc.The metal and ceramic gradient material is the high performance material that a kind of component, structure, physical parameter are continuous variation or stepped change, requires the sintering temperature of each layer also different, utilizes traditional sintering method to be difficult to once-firing.The SPS sintering can be used stair-stepping graphite jig, owing to the different thermogrades that produce of mould upper and lower end current density, satisfies the sintering of the different functionally gradient material (FGM) of composition proportion.But its thermograde direction is single, is not suitable for the sintering of powder particle gradient composite powder.The composite powder sintering of nano ceramic powder clad metal or alloying pellet does not appear in the newspapers as yet.
Summary of the invention
The objective of the invention is the metal alloy powders of surperficial clad nano ceramic powders is utilized a kind of micelle ceramic/metal block composite material of discharge plasma sintering method preparation and preparation method thereof.
The institutional framework of described micelle ceramic/metal block composite material: the composite construction that micelle ceramic/metallic composite is made up of metal or alloy in cellular sealing micelle ceramic and the born of the same parents, micelle ceramic granularity are 5～90 microns, 1～2 micron of cell wall wall thickness.The ceramic sintered bodies of the densification that cell wall is made up of ceramic cladding powder; Be the basic powder of elemental metals or two kinds of above alloys of constituent element in the born of the same parents, it is evenly tiny that alloy organizing keeps.
This institutional framework characteristics help keeping many physics and chemistry that component had and the mechanical performance characteristic in the sample.Because the alloy cell space sealed by complete ceramic cell wall, so ceramic wear-resisting, high temperature resistant, anticorrosive, characteristic such as anti-oxidant will embody in this composite construction.The performance of the ceramic phase in composite is showed fully.Because ceramic layer constitutes space sealing cell structure, has isolated the contact between the metal in the born of the same parents fully, has suppressed the diffusion of the atom between the contiguous cell space, alloy grain is grown up be restricted, and has comprehensive mechanical performance preferably.
The technology of preparing scheme of described micelle ceramic/metal block composite material is:
The preparation process of micelle ceramic/metal block composite material comprises the preparation and the discharge plasma sintering of the composition design of alloy powder and preparation, the compound base of colding pressing, and its process is:
1) selection of composition
The cost and the performance of material mainly considered in the selection of material composition.Performance is meant mechanical performance and functional (as the physicochemical properties such as electric conductivity, thermal conductivity, resistance to elevated temperatures, resistance to chemical corrosion, magnetic properties) that composite is required.Can consider that selecting the elemental metals of metal blocks or alloy basis powder size is 5～90 microns from various physicochemical properties and mechanical performance collocation; Selecting the ceramic cladding powder granularity of micelle ceramic is the Al of 5～90 nanometers
2O
3Or ZrO
2Ceramic material.
2) preparation of the compound base of colding pressing
With metal or alloy basis powder and ceramic cladding powder (9～20) by volume: 1 mixes, and is ground to the nanometer cladding powder with agate mortar and fully evenly is coated on basic powder surface, carries out the SPS sintering after putting into mold cold compression set type.
3) discharge plasma sintering is densified
Adopt the discharge plasma sintering system, with the sintering condition of metal or alloy powder particle serve as the basis by corresponding pressure, temperature, the sintering current sintering condition, the densification sintering that carries out composite powder is shaped.
The beneficial effect of the technology of the present invention:
1. the technology that technical scheme of the present invention prepares born of the same parents' shape ceramic/metal block composite material is simple, easy to operate, sintering process sequencing control.
2. adopt the special composite mode of born of the same parents' shape ceramic/metal composite materials of technical solution of the present invention preparation to make its performance characteristics, and the characteristics that the adjustment collocation by raw material components has this structural composite material in the scope of unusual tolerance: to help keeping many physics and chemistry that component had and mechanical performance characteristic in the sample with the not available pottery of conventional metals based composites.Because the alloy cell space sealed by complete ceramic cell wall, so ceramic wear-resisting, high temperature resistant, anticorrosive, characteristic such as anti-oxidant will embody in this composite construction.The performance of the ceramic phase in composite is showed fully.Because ceramic layer constitutes space sealing cell structure, has isolated the contact between the metal in the born of the same parents fully, has suppressed the diffusion of the atom between the contiguous cell space, alloy grain is grown up be restricted, and has comprehensive mechanical performance preferably.
Description of drawings
Fig. 1 is a sintering parameter schematic diagram.
Fig. 2 is Al
2O
3The SEM photo of nanometer powder.
Fig. 3 is Al
2O
3The XRD curve of nanometer powder.
Fig. 4 is the SEM photo of AlMnCe alloy powder.
Fig. 5 is the XRD curve of AlMnCe alloy powder.
Fig. 6 is Al
2O
3Nano powder and AlMnCe mixed powder for alloy grind the SEM photo of the composite powder of back formation.
Fig. 7 is the SEM photo of born of the same parents' shape ceramic/metal composite materials behind the sintering.
Fig. 8 is the compression curve of born of the same parents' shape ceramic/metal composite materials sample.
The specific embodiment
The present invention is a kind of micelle ceramic/metal block composite material of utilizing the discharge plasma sintering method preparation of the metal alloy powders with surperficial clad nano ceramic powders and preparation method thereof.
The institutional framework of described micelle ceramic/metal block composite material: the composite construction that micelle ceramic/metallic composite is made up of metal or alloy in cellular sealing micelle ceramic and the born of the same parents, micelle ceramic granularity are 5～90 microns, 1～2 micron of cell wall wall thickness.The ceramic sintered bodies of the densification that cell wall is made up of ceramic cladding powder; Be the basic powder of elemental metals or two kinds of above alloys of constituent element in the born of the same parents, it is evenly tiny that alloy organizing keeps.
This institutional framework characteristics help keeping many physics and chemistry that component had and the mechanical performance characteristic in the sample.Because the alloy cell space sealed by complete ceramic cell wall, so ceramic wear-resisting, high temperature resistant, anticorrosive, characteristic such as anti-oxidant will embody in this composite construction.The performance of the ceramic phase in composite is showed fully.Because ceramic layer constitutes space sealing cell structure, has isolated the contact between the metal in the born of the same parents fully, has suppressed the diffusion of the atom between the contiguous cell space, alloy grain is grown up be restricted, and has comprehensive mechanical performance preferably.
The technology of preparing scheme of described micelle ceramic/metal block composite material is:
The preparation process of micelle ceramic/metal block composite material comprises the preparation and the discharge plasma sintering of the composition design of alloy powder and preparation, the compound base of colding pressing, and its process is:
1) selection of composition
The cost and the performance of material mainly considered in the selection of material composition.Performance is meant mechanical performance and functional (as the physicochemical properties such as electric conductivity, thermal conductivity, resistance to elevated temperatures, resistance to chemical corrosion, magnetic properties) that composite is required.Can consider that selecting the basic powder size of metal or alloy in the born of the same parents is 5～90 microns from various physicochemical properties and mechanical performance collocation; Selecting the ceramic cladding powder granularity of micelle ceramic is the Al of 5～90 nanometers
2O
3Or ZrO
2Ceramic material.
2) preparation of the compound base of colding pressing
With metal or alloy basis powder and ceramic cladding powder (9～20) by volume: 1 mixes, and is ground to the nanometer cladding powder with agate mortar and fully evenly is coated on basic powder surface, carries out the SPS sintering after putting into mold cold compression set type.
3) discharge plasma sintering is densified
Adopt the discharge plasma sintering system, with the sintering condition of metal or alloy powder particle serve as the basis by corresponding pressure, temperature, the sintering current sintering condition, the densification sintering that carries out composite powder is shaped.
Illustrated for example below.
Al, the Mn and the Ce that with purity are 99.97wt% are raw material, are Al with arc melting
90Mn
9Ce
1The alloy spindle is then with high pressure gas atomizing method spray alloy powder.It is stand-by to get granularity powder between 25～45 microns. get Al
90Mn
9Ce
1The Al of atomized powder and wet chemistry method preparation
2O
3Nano powder mixes by 10: 1 (weight ratio), grinds with agate mortar and makes Al
2O
3Nano powder all evenly is coated on Al
90Mn
9Ce
1The atomized powder surface, the laggard capable SPS sintering of the base of colding pressing.The SPS experiment is carried out on the SPS-1050 of Sumitomo company type discharge plasma sintering machine, uses graphite jig, former intracavity diameter 20mm.Be placed with graphite paper between former and the formpiston and between formpiston and the sample, make galvanic couple thermometer hole and sample be centered close to sustained height behind the pretension, guarantee that thermometric is true and reliable.The control of sintering parameter is temperature-temporal mode, the 6Pa argon gas atmosphere, and sintering current is to be restricted by temperature schedule, the SPS system is given automatically, degas at 200 ℃ of insulation 3min, be warmed up to 520 ℃ (average sintering current are 1000A) with 1min again, insulation 3min (during electric current be 600A).Vertical uniaxial tension 50MPa of formpiston remains in whole sintering process (concrete parameter as shown in Figure 1).Adopt Al
90Mn
9Ce
1(atomic percentage) alloy powder respectively with the Al of 10,50,60,80 or 90 nanometers
2O
3The powder mixed sintering.The discharge plasma sintering process parameter is synthesized sintering in the SPS-1050 type discharge plasma sintering system as shown in Figure 1.Al
90Mn
9Ce
1SEM pattern such as Fig. 2 of virgin alloy powder, XRD analysis result as shown in Figure 3, Al
2O
3The SEM pattern of nano powder as shown in Figure 4, the XRD curve is as shown in Figure 5.Mixed grinding form by the pattern of coating compound powder as shown in Figure 6, the micella Al that forms behind the sintering
2O
3Pottery/Al
90Mn
9Ce
1The institutional framework of alloy composite materials sample is Al about 1 micron by thickness
2O
3Al in pottery cell wall and the born of the same parents
90Mn
9Ce
1Alloy constitutes (as shown in Figure 7).Sample has the high compressive strength of 514MPa and 0.65% high residual pressure shrinkage (as shown in Figure 8).
Claims (2)
1. micelle ceramic/metal block composite material, it is characterized in that: the institutional framework of described micelle ceramic/metal block composite material: the composite construction that micelle ceramic/metallic composite is made up of metal or alloy in cellular sealing micelle ceramic and the born of the same parents, the micelle ceramic granularity is 5～90 microns, the cell wall wall thickness is 1～2 micron, be the basic powder of the alloy of elemental metals or two or more constituent elements in the born of the same parents, it is evenly tiny that alloy organizing keeps; And the ceramic sintered bodies of the densification that sealing micelle ceramic cell wall is made up of ceramic cladding powder, ceramic cladding powder is Al
2O
3Or ZrO
2Ceramic material.
2. the preparation method of the described micelle ceramic/metal block composite material of claim 1, it is characterized in that: the preparation process of described micelle ceramic/metal block composite material comprises the preparation and the discharge plasma sintering of the one-tenth component selections of alloy powder and preparation, the compound base of colding pressing, and its process is:
1) selection of composition
The cost and the performance of material mainly considered in the selection of material composition, considers that from various physicochemical properties and mechanical performance collocation selecting the basic powder size of metal or alloy in the born of the same parents is 25～45 microns; Selecting the ceramic cladding powder granularity of micelle ceramic is the Al of 5～90 nanometers
2O
3Powder or ZrO
2Ceramic material;
2) preparation of the compound base of colding pressing
With above-mentioned metal or alloy basis powder and ceramic cladding powder (9～20) by volume: 1 mixes, and is ground to ceramic powders with agate mortar and fully evenly is coated on basic powder surface, carries out the SPS sintering after putting into mold cold compression set type;
3) discharge plasma sintering is densified: adopt the discharge plasma sintering system, with the sintering condition of metal or alloy powder particle serve as the basis by corresponding pressure, temperature, the sintering current sintering condition, the densification sintering that carries out composite powder is shaped.
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| CN1304195C true CN1304195C (en) | 2007-03-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100453212C (en) * | 2007-07-17 | 2009-01-21 | 南京航空航天大学 | Mechanical process of preparing composite nanometer ceramic and micron metal powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113149688B (en) * | 2020-01-23 | 2022-12-09 | 上海交通大学 | Composite ceramic with honeycomb fiber structure and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000128630A (en) * | 1998-10-27 | 2000-05-09 | Asahi Optical Co Ltd | Ceramic composite and its production |
| CN1371885A (en) * | 2002-04-01 | 2002-10-02 | 武汉理工大学 | Preparation of aluminium nitride transparent ceramics by discharge plasma sintering method |
| JP2002309323A (en) * | 2001-04-12 | 2002-10-23 | Toyama Prefecture | Functionally gradient material composed of low-melting point metal and oxide ceramics, and its manufacturing method |
| CN1382660A (en) * | 2002-06-19 | 2002-12-04 | 北京工业大学 | Composite Ti-HA material and its preparing process |
-
2004
- 2004-12-14 CN CNB2004100971967A patent/CN1304195C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000128630A (en) * | 1998-10-27 | 2000-05-09 | Asahi Optical Co Ltd | Ceramic composite and its production |
| JP2002309323A (en) * | 2001-04-12 | 2002-10-23 | Toyama Prefecture | Functionally gradient material composed of low-melting point metal and oxide ceramics, and its manufacturing method |
| CN1371885A (en) * | 2002-04-01 | 2002-10-02 | 武汉理工大学 | Preparation of aluminium nitride transparent ceramics by discharge plasma sintering method |
| CN1382660A (en) * | 2002-06-19 | 2002-12-04 | 北京工业大学 | Composite Ti-HA material and its preparing process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100453212C (en) * | 2007-07-17 | 2009-01-21 | 南京航空航天大学 | Mechanical process of preparing composite nanometer ceramic and micron metal powder |
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