CN102560178A - Method for preparing porous material - Google Patents
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- CN102560178A CN102560178A CN2012100383616A CN201210038361A CN102560178A CN 102560178 A CN102560178 A CN 102560178A CN 2012100383616 A CN2012100383616 A CN 2012100383616A CN 201210038361 A CN201210038361 A CN 201210038361A CN 102560178 A CN102560178 A CN 102560178A
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Abstract
The invention discloses a method for preparing a porous material, and relates to the fields of material processing, mechanical manufacturing and the like. The method comprises the following steps of: heating particles of metal or ceramic powder serving as a raw material until the surfaces of the particles are micro-melted or semi-melted, heating a substrate to certain temperature, and preparing a porous coating or block. The material which is prepared by the method and has a porous structure is wide in raw material selection range and pore range and controllable in pore size structure, mechanical property and surface state, and coatings or blocks with different thickness can be obtained according to requirements. The method is a new method for preparing the porous material through thermal spraying.
Description
Technical field
The present invention relates to fields such as materials processed, machinofacture; The preparation method who relates to porous material, this method especially are fit to low-cost preparation fast porosity is adjustable, pore dimension is controlled, mechanical property is controlled, condition of surface is controlled block body stephanoporate material or coating porous material.
Background technology
Porous material has the excellent specific property of structure, function integration, is a kind of critical material in the national economic development.On the structure, porous material has characteristics such as density is little, specific surface area is big; On the function, porous material has multiple performances such as vibration damping, damping, sound-absorbing, sound insulation, heat radiation, absorption striking energy, electromagnetic shielding.Because abundant pore morpholohy, bigger aperture ranges; Porous material is used and is spreaded all over every field such as aerospace, war industry, building, electronic communication, communications and transportation, biomedicine, electrochemistry, machinery, metallurgy, energy environment protection; Can be used as vibroshock, snubber, energy absorber, strainer, fluid through the cooling transpiring material of exhaust snubber, support of the catalyst, porous metal electrode, rocket nose cone and the empennage of device, heat exchanger, flash arrestor, mover, the sound damper of underwater submarine etc., have the status of not replacing in the materialogy field.
Traditional porous material preparation method can be divided into following several big type substantially: 1, based on the method for metal melt; 2, based on the method for metal-powder; 3, based on the method for metal vapors; 4, based on the method for metals ion.But these technologies of preparing generally all exist the deficiency of aspects such as technology, cost.Thermospray is as a kind of surface strengthening technology, has on practical applications that the material range of choice is wide, low cost, high-level efficiency, is convenient to plurality of advantages such as control.Hot spray coating is partly connected and is piled up by flat particle and constitutes; Unavoidably there is the space in coating inside; Be generally 0.5%～20%,, added pore-forming material (such as organism or inorganics that can follow-up place to go) in the spray material in the past in order to increase porosity; Yet resulting porosity still is difficult to significantly improve.U.S. Pat 4542539 adopted the little molten titanium valve particle of flame plating deposition surface in 1985; The titanium valve grain diameter is reduced to coatingsurface by matrix gradually, prepares porous gradient titanium coating with this thinking, and anchoring strength of coating is low; Only 7MPa, and complex process.The Kobe Steel company of Japan adopts vacuum plasma spray coating (VPS), ti powder is accelerated under the fritting state deposit in plasma flame flow, thereby prepares porosity 40～60%, compressive strength is the porous titanium coating of 85MPa.In the world also some document (like S.Endres et al.; Correlation of in vitro and in vivo results of vacuum plasmasprayed titanium implants with different surface topography; J Mater Sci:Mater Med (2008) 19:1117-1125) VPS is prepared Ti and the Ti alloy coat is reported; Coating porosity homogeneity and the perforate connectedness prepared are relatively poor; Porosity distribution is narrower, only aspect artificial skelecton, uses to some extent.In addition; The vacuum plasma spray coating apparatus expensive; The patent CN2005100211694.8 of China Sichuan University attempts adopting the method for air plasma spraying and atmosphere protection; The method of the cold spraying post-heat-treated that CN200810018199.5 adopted of Northwestern Polytechnical University's application prepares Ti to vacuum cold spray under the performance prerequisite that guarantees coating and the Ti alloy coat replaces, but all can't the method for original vacuum plasma be surmounted.In addition; Also there is few patents that other material is reported; CN200710137112.1 has described a kind of preparation method who produces the capillary structure of soaking plate with high temperature powder spray gun; Material therefor is a copper powder, and aluminium powder or other powder are heated to the molten state of surface micro through high temperature powder spray gun with powder particle and amass at the enterprising windrow of cold metal plate.Up to now; Both at home and abroad molten or fritting deposition method successfully prepares the report of porous material and few with this kind surface micro; And the overwhelming majority only concentrates on the preparation titanium or titanium alloy coating, and tracing it to its cause is because the dusty spray particle is in fritting particularly during the molten state deposit of surface micro; If fusing degree and sedimentation velocity do not form matching relationship, then can reduce sedimentation effect so that coating greatly and be difficult to form.
Summary of the invention
Defective or deficiency to above-mentioned technology existence; The objective of the invention is: provide a kind of and prepare the method for porous material based on thermospray, the selectable material ranges of porous coating that this method is prepared or material is wide, the void distribution controlled range is big, pore texture is even, sedimentation effect is high.
General technical thinking of the present invention is: based on heat spraying method, through matrix is heated to high temperature, and adopt lower particle speed, the bounce-back and the tendency of breakking away when reducing the fritting particle deposition, and then the novel preparation method of porous material.Through selecting suitable processing parameter, flight velocity and melted state during control spraying particle deposition make to deposit under the condition of particle or partial melting molten in surface micro and add up, and realize the method for porous material preparation.The core of this kind porous metal material moulding is that the stickiness melt portions through the fritting particle realizes intergranular bridge joint, and the rigid element of fritting particle forms stephanoporate framework, between rigid particles not contact part form hole.Particularly spraying particle is under the molten state of surface micro, because the spraying particle deposition has single direction property, deposited particles can cause follow-up particle and " block " effect on the space, in the hope of forming big hole, thereby increases substantially the porosity of coating.Characteristic (size distribution of compaction rate, powder, the shape of powder etc.) through the adjustment powder comes porosity and pore texture are adjusted.This kind method is along the characteristics of holding heat spraying method, and it is simple to be used for preparing porous material technology, and efficient is high, and energy expenditure is low, and preparation parameter is easy to control, and good reproducibility is easy to realize the preparation of the perforate/closed pore unitized construction of different porosities.
The present invention is achieved through following technical proposals:
A kind of preparation method of porous material, carry out as follows:
(1) the powder particle heating with porous material makes it form surface melting and the solid-state fritting particle of inner maintenance;
(2) matrix surface is heated to depositing temperature; Depositing temperature is 200～1500 ℃; Make above-mentioned fritting particle collision deposit to matrix surface; Keeping the sedimental surface temperature of institute's formation of deposits then is above-mentioned depositing temperature, continues to make the fritting particle deposition that adds up, between the fritting particle owing to incomplete filling effect form size less than or be equivalent to the small scale hole of powder particle;
(3) through control fritting particle surface fusing degree and speed; The contact interface position that liquid portion flow to arrive this fritting particle and matrix surface forward when making the fritting particle collision to matrix surface and solidify forms effective combination the between this fritting particle and the deposition surface on every side;
(4) through the control particle speed, solidify the in-situ deposition of realizing collision through liquid when making particle collision to deposition surface, rather than significantly towards front slide, backwards or the side bounce-back; Form the bridging effect of particle downsides through a plurality of particulate random deposition, thereby obtain size significantly greater than the big scale hole of powder particle.
Described fritting particle obtains through following method: a kind of refractory grain material and another kind of low melting material are constituted matrix material, it heat in thermal source make surface that low melting material fusing back forms with low-melting-point liquid and inside remains solid-state fritting particle.
When said porous material was organism, metal or alloy, its depositing temperature was 0.3～0.5 times of fusing point; Said porous material is organism or metal or alloy when being the matrix material of external phase, and its depositing temperature is 0.3～0.5 times of fusing point; When said porous material was inorganic non-metallic, its depositing temperature was at 0.4～0.6 times of fusing point.
The thickness of the described smelting zone that starts from the fritting particle surface between one of percentage of equivalent particle diameter to nearly 2/3rds.
During the collision of described fritting particle and matrix, near the melt portions that is in the fritting particle surface flows to contact area along the fritting particle surface, and the solid granulates part formed firm being connected with the fritting particle at impact point place through liquid phase.
Described powder particle constitutes through the mode of partially filled or completely filled as skeleton and in its hole inside and has the more porous material of small scale hole.
One or more modes heat described powder particle in combustion flame, plasma, electric arc, laser, the induction through adopting.
Described high temperature adopts the thermal source of heated particle or adopts flame, electric arc, plasma, laser, induction, electric heating, in infrared one or more to heat.
The mean sizes of described powder particle is from several microns to hundreds of microns;
The size-grade distribution of described powder particle is between the scope of average plus-minus 20%;
The granularity of described powder particle is that unimodal distribution or multimodal distribute;
Described fritting particulate speed is in the scope of number m/s to 100m/s, and particle deposits on matrix surface with lower kinetic collision;
Described powder particle is single oxide compound, carbide, nitride, silicide ceramics particle;
Described powder particle is single metal or alloy;
Described powder particle is mixing material or the matrix material that the close metal of fusing point and metal, Metal and Alloy, alloy and alloy, pottery and pottery constitute;
Described powder particle is full particle or hollow bead;
The thickness of the surface melting layer that described fritting particle is a hollow bead is less than shell thickness.
The hole of described porous material is 10%～99%;
Described porous material is porous coating or porous bulk, and thickness range is at tens microns to several centimetres;
Described fritting particulate sedimentary environment is an air atmosphere
Protection of inert gas atmosphere or vacuum that described fritting particulate sedimentary environment is;
Described porous material carries out post-heat-treated or reduction as requested, and composition, the mechanical property of porous material are adjusted improvement.
The porous material of method preparation of the present invention is applicable to general dusty spray material; Few to the material requirements restriction, low-cost preparation fast porosity is adjustable, pore dimension is controlled, mechanical property is controlled, condition of surface is controlled block body stephanoporate material or coating porous material.
Description of drawings
Fig. 1: the starting powder pattern photo that embodiment of the present invention is related, wherein (a) is the YSZ (ZrO that handles rear section hollow through plasma spheroidization
2+ 8mol.%Y
2O
3) powder, (b) be high-density Mo powder, (c) be the Ni50Cr50 powdered alloy, (d) be the Ni powder.
Fig. 2: the porous material weave construction that the YSZ powder of employing Fig. 1 (a) makes, (a) be surface topography, (b) be the polishing fractography after strike-through is handled.
Fig. 3: porous material macro morphology and microtexture that the Mo powder of employing Fig. 1 (b) makes (a) are spraying attitude exterior appearance, (b) for spraying attitude surface topography, (c) for going back the ortho states exterior appearance, (d) for going back the ortho states cross-section morphology.
Fig. 4: the fractography (a) of the porous Mo of present technique preparation (b), surface topography (c) is (d) and the fractography of effective calmodulin binding domain CaM of particle junction (e).(a) be lithosomic body polishing fractography and local enlarged photograph, under the blocking of a series of directed stacking particles, form big hole (black part), the length of a certain dimension of hole can reach the diameter of tens particles; (b) be local enlarged photograph in (a), form some little holes closely between particle cluster bunch at some stackings, these little holes are separated by interparticle linking neck, and size is at tens microns; (c) be the local enlarged photograph of the surface topography of section, the collision of a fritting particle inclination is deposited on the sedimentary particle, and the diameter that connects neck can reach the diameter of the solid-state part of fritting particle; (d) be the local enlarged photograph of surface topography; Two particles forms neck and connects; When fritting particle collision during to deposition surface (promptly going up a particle); The control particle speed is low to make liquid part flow to that the granular boundary place promptly solidifies rather than flows forward significantly again and leave at the interface, connects forming effectively at the interface thus, and this figure shows that the big I of neck reaches the half the of fusing back particle; (e) be the polishing section photo that connects particle like two levels in (d), the original surface before the particle encounter disappears, and shows to have formed good binding between particle.
Fig. 5: the porous material surface pattern that the Ni50Cr50 powder of employing Fig. 1 (c) makes, (a) acetylene flow 250L/h, (b) acetylene flow 400L/h.
Fig. 6: the porous material weave construction for the Ni powder that adopts Fig. 1 (d) makes, (a) be surface topography, (b) be the polishing fractography after the strike-through processing.
Embodiment
Below be the specific embodiment that the contriver provides, need to prove that these embodiment are the more excellent examples of the present invention, be used for those skilled in the art and understand the present invention, but the present invention is not limited to these embodiment.
Embodiment 1:
With flame plating YSZ powder is example, part powder hollow, powder diameter 30～40 μ m.Used flame spray gun is a QT-E2000-7/h type oxy-acetylene powered guns.Flame gun is through the Motoman Robot actions, and walking rifle speed is 100mm/s.Spraying adopts oxygen to carry out powder feeding, and acetylene flow 360L/h, spray distance are 20mm, and flame is the low-level oxidation flame, and compressed air require is 1500L/h.The YSZ base sheet of φ 30 (dusty spray compacting back sintering is formed) is heated under 1000 ℃ the condition and sprays, with infrared infrared thermometer (RAYRPM30L3U, Raytek, USA) surface temperature before the monitoring matrix, the maintenance homo(io)thermism is at about 1000 ℃.The bump matrix surface was realized deposition after flame was heated to powder the state of surface melting, thereby formed the YSZ porous material.
Embodiment 2:
Change the YSZ powder among the embodiment 1 the Mo powder of 75～100 μ m into, the acetylene flow is 300L/h, spray distance 30mm.Matrix is the nickel base superalloy sheet of φ 20, and substrate temperature is controlled at 800 ℃.Other conditions all remain unchanged.For obtaining purified Mo porous material, will spray the attitude porous material and at high temperature reduce in the atmosphere of hydrogen.The bump matrix surface was realized deposition after flame was heated to powder the state of surface melting, thereby formed the Mo porous material.
Embodiment 3:
Change the YSZ powder among the embodiment 1 the Ni50Cr powder of 75～100 μ m into, the acetylene flow is 250L/h and 400L/h, and spray distance is 20mm.Matrix is the nickel base superalloy sheet of φ 20, and substrate temperature is controlled at 400 ℃.Other conditions all remain unchanged.The bump matrix surface was realized deposition after flame was heated to powder the state of surface melting, thereby formed the Ni50Cr porous material.
Embodiment 4:
Change the YSZ powder among the embodiment 1 the Ni powder of 100～125 μ m into, the acetylene flow is 200L/h, and spray distance is 20mm.Matrix is the nickel base superalloy sheet of φ 20, and substrate temperature is controlled at 400 ℃.Other conditions all remain unchanged.The bump matrix surface was realized deposition after flame was heated to powder the state of surface melting, thereby formed the Ni porous material.
Embodiment 5:
Adopting the plasma spraying particle diameter is the Mo coating of bimodal distribution, is respectively 75～100 μ m and 200～250 μ m, uniform mixing, and stainless steel is made base sheet, and substrate temperature remains on 800 ℃.The bump matrix surface was realized deposition after flame was heated to powder the state of surface melting, thereby formed the Mo porous material.
Embodiment 6:
Adopting the plasma spraying particle diameter is the hollow YSZ powder of 75～100 μ m, and the diameter of hollow parts is the half the of powder diameter, and stainless steel is made base sheet, and substrate temperature remains on 1000 ℃.The bump matrix surface was realized deposition after flame was heated to powder the state of surface melting, thereby formed the YSZ porous material.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction; Though the present invention discloses as above with preferred embodiment; Yet be not in order to limiting the present invention, anyly be familiar with the professional and technical personnel, in not breaking away from technical scheme scope of the present invention; When the method for above-mentioned announcement capable of using and technology contents are made a little change or be modified to the equivalent embodiment of equivalent variations; In every case be the content that does not break away from technical scheme of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (10)
1. the preparation method of a porous material is characterized in that, carries out as follows:
(1) the powder particle heating with porous material makes it form surface melting and the solid-state fritting particle of inner maintenance;
(2) matrix surface is heated to depositing temperature; Depositing temperature is 200～1500 ℃; Make above-mentioned fritting particle collision deposit to matrix surface; Keeping the sedimental surface temperature of institute's formation of deposits then is above-mentioned depositing temperature, continues to make the fritting particle deposition that adds up, between the fritting particle owing to incomplete filling effect form size less than or be equal to the small scale hole of powder particle;
(3) through control fritting particle surface fusing degree and speed; The contact interface position that liquid portion flow to arrive this fritting particle and matrix surface forward when making the fritting particle collision to matrix surface and solidify forms effective combination the between this fritting particle and the deposition surface on every side;
(4) through the control particle speed, solidify the in-situ deposition of realizing collision through liquid when making particle collision to deposition surface, rather than significantly towards front slide, backwards or the side bounce-back; Form the bridging effect of particle downsides through a plurality of particulate random deposition, thereby obtain size significantly greater than the big scale hole of powder particle.
2. the preparation method of porous material according to claim 1 is characterized in that:
Described fritting particle obtains through following method: a kind of refractory grain material and another kind of low melting material are constituted matrix material, it heat in thermal source make surface that low melting material fusing back forms with low-melting-point liquid and inside remains solid-state fritting particle.
3. the preparation method of porous material according to claim 1 is characterized in that:
When said porous material was organism, metal or alloy, its depositing temperature was 0.3～0.5 times of fusing point; Said porous material is organism or metal or alloy when being the matrix material of external phase, and its depositing temperature is 0.3～0.5 times of fusing point; When said porous material was inorganic non-metallic, its depositing temperature was at 0.4～0.6 times of fusing point.
4. the preparation method of porous material according to claim 1 is characterized in that:
The thickness of the described smelting zone that starts from the fritting particle surface between one of percentage of equivalent particle diameter to nearly 2/3rds.
5. the preparation method of porous material according to claim 1 is characterized in that:
During the collision of described fritting particle and matrix, near the melt portions that is in the fritting particle surface flows to contact area along the fritting particle surface, and the solid granulates part formed firm being connected with the fritting particle at impact point place through liquid phase.
6. the preparation method of porous material according to claim 1 is characterized in that:
Described powder particle constitutes through the mode of partially filled or completely filled as skeleton and in its hole inside and has the more porous material of small scale hole.
7. the preparation method of porous material according to claim 1 is characterized in that:
One or more modes heat described powder particle in combustion flame, plasma, electric arc, laser, the induction through adopting.
8. the preparation method of porous material according to claim 1 is characterized in that:
Described high temperature adopts the thermal source of heated particle or adopts flame, electric arc, plasma, laser, induction, electric heating, in infrared one or more to heat.
9. the preparation method of porous material according to claim 1 is characterized in that:
The mean sizes of described powder particle is from several microns to hundreds of microns;
The size-grade distribution of described powder particle is between the scope of average plus-minus 20%;
The granularity of described powder particle is that unimodal distribution or multimodal distribute;
Described fritting particulate speed is in the scope of 0m/s to 100m/s, and particle deposits on matrix surface with lower kinetic collision;
Described powder particle is single oxide compound, carbide, nitride or silicide ceramics particle;
Described powder particle is single metal or alloy;
Described powder particle is mixing material or the matrix material that the close metal of fusing point and metal, Metal and Alloy, alloy and alloy, pottery and pottery constitute;
Described powder particle is full particle or hollow bead;
The thickness of the surface melting layer that described fritting particle is a hollow bead is less than shell thickness.
10. the preparation method of porous material according to claim 1 is characterized in that:
The hole of described porous material is 10%～99%;
Described porous material is porous coating or porous bulk, and thickness range is at tens microns to several centimetres;
Described fritting particulate sedimentary environment is an air atmosphere;
Protection of inert gas atmosphere or vacuum that described fritting particulate sedimentary environment is;
Described porous material carries out post-heat-treated or reduction as requested, and composition, the mechanical property of porous material are adjusted improvement.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103103473A (en) * | 2013-02-05 | 2013-05-15 | 西安交通大学 | Method for preparing erosion resistive and high-temperature abradable seal coating based on hot spraying |
| CN104782616A (en) * | 2015-04-21 | 2015-07-22 | 西安交通大学 | Application of porous metal material to biological sample freezing and freezing method |
| CN105603356A (en) * | 2016-03-30 | 2016-05-25 | 西安交通大学 | Metal coating with high bonding strength and high cohesion strength, as well as thermal spraying method and application of metal coating |
| CN105642885A (en) * | 2016-03-30 | 2016-06-08 | 西安交通大学 | Thermal spraying self-bonding metal alloy powder with coated composite structure |
| CN108085643A (en) * | 2017-12-14 | 2018-05-29 | 东北大学 | A kind of damping coatings for being formed at metal part surface and preparation method thereof |
| CN108698123A (en) * | 2015-12-30 | 2018-10-23 | 莫特公司 | Multiple-Aperture Device made of laser gain material manufacture |
| CN110408950A (en) * | 2019-08-30 | 2019-11-05 | 南通大学 | A kind of electrolysis water cathode and preparation method thereof based on microcosmic blasting technology |
| CN111273750A (en) * | 2018-12-04 | 2020-06-12 | 广州力及热管理科技有限公司 | Capillary structure element |
| CN111964500A (en) * | 2020-07-08 | 2020-11-20 | 广东工业大学 | Method for preparing flexible micro heat pipe by laser-induced reduction sintering of copper oxide ink |
| CN114574798A (en) * | 2022-04-02 | 2022-06-03 | 华东理工大学 | Design and preparation method of high-strain-tolerance anti-sintering thermal barrier coating structure |
| CN115229188A (en) * | 2022-06-24 | 2022-10-25 | 广东省科学院新材料研究所 | Porous metal material and manufacturing method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103103473A (en) * | 2013-02-05 | 2013-05-15 | 西安交通大学 | Method for preparing erosion resistive and high-temperature abradable seal coating based on hot spraying |
| CN104782616A (en) * | 2015-04-21 | 2015-07-22 | 西安交通大学 | Application of porous metal material to biological sample freezing and freezing method |
| CN108698123A (en) * | 2015-12-30 | 2018-10-23 | 莫特公司 | Multiple-Aperture Device made of laser gain material manufacture |
| CN105642885A (en) * | 2016-03-30 | 2016-06-08 | 西安交通大学 | Thermal spraying self-bonding metal alloy powder with coated composite structure |
| CN105603356B (en) * | 2016-03-30 | 2018-09-04 | 西安交通大学 | High bond strength and cohesive strength metal coating and thermal spraying preparation method and application |
| CN105603356A (en) * | 2016-03-30 | 2016-05-25 | 西安交通大学 | Metal coating with high bonding strength and high cohesion strength, as well as thermal spraying method and application of metal coating |
| CN105642885B (en) * | 2016-03-30 | 2018-10-30 | 西安交通大学 | A kind of thermal spraying self-adhesive metal alloy powders with covered composite yarn structure |
| CN108085643A (en) * | 2017-12-14 | 2018-05-29 | 东北大学 | A kind of damping coatings for being formed at metal part surface and preparation method thereof |
| CN111273750A (en) * | 2018-12-04 | 2020-06-12 | 广州力及热管理科技有限公司 | Capillary structure element |
| CN110408950A (en) * | 2019-08-30 | 2019-11-05 | 南通大学 | A kind of electrolysis water cathode and preparation method thereof based on microcosmic blasting technology |
| CN110408950B (en) * | 2019-08-30 | 2021-04-27 | 南通大学 | Electrolytic water cathode based on microscopic blasting process and preparation method thereof |
| CN111964500A (en) * | 2020-07-08 | 2020-11-20 | 广东工业大学 | Method for preparing flexible micro heat pipe by laser-induced reduction sintering of copper oxide ink |
| CN114574798A (en) * | 2022-04-02 | 2022-06-03 | 华东理工大学 | Design and preparation method of high-strain-tolerance anti-sintering thermal barrier coating structure |
| CN115229188A (en) * | 2022-06-24 | 2022-10-25 | 广东省科学院新材料研究所 | Porous metal material and manufacturing method and application thereof |
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