CN104759630A - Preparation method of porous metal foil - Google Patents
Preparation method of porous metal foil Download PDFInfo
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- CN104759630A CN104759630A CN201510153106.XA CN201510153106A CN104759630A CN 104759630 A CN104759630 A CN 104759630A CN 201510153106 A CN201510153106 A CN 201510153106A CN 104759630 A CN104759630 A CN 104759630A
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Abstract
The invention discloses a preparation method of a porous metal foil. The porous metal foil is a thin sheet manufactured from metal porous materials. The method comprises the steps of (1) preparing raw powder for preparing the metal porous material into thick suspension through a dispersing agent and adhesive; (2) pouring the suspension into a forming die cavity of a file preparing tool, and drying to form a homogenized film; (3) pressing the film to improve the accumulation density of powder particles in the film; (4) sintering the pressed film to obtain the porous metal foil. According to the method, the pressing can improve the accumulation density of the powder particle in the film, and the average diameter of the flexible porous metal foil can reduced and uniform; the pressing pressure can be selected to control the average diameter of the flexible porous metal foil.
Description
Applicant of the present invention have submitted on October 31st, 2014 that application number is 2014106089803, the application for a patent for invention of title " flexible, porous metal forming and preparation method thereof ".There is provided DE flexible, porous metal forming and preparation method thereof may there is technical association with the application in the description of this earlier application.Because this earlier application is not yet open in the applying date of the application, therefore the content related in the following content of this description in this earlier application more so that the public read present specification time can more comprehensive, have a clear understanding of this flexible, porous metal forming and technology of preparing thereof.
Technical field
The present invention relates to sintering diamond bit and preparation thereof, be specifically related to the preparation method of flexible, porous metal forming and flexible, porous metal forming.
Background technology
The main of sintering diamond bit is used as filtering material.In a particular application, sintering diamond bit need be made the filter element of definite shape and structure, then filter element is installed in filter.Existing sintering diamond bit filter element is all cast or the plate profile structure of rigidity substantially.Their preparation principle is similar, namely be haply: the pressed compact (generally adopting equal pressing forming technology) first by special mould, the raw meal forming this metal polyporous material being pressed into cast or template, and then pressed compact is sintered, obtain product after sintering.
The sintering diamond bit filter element of above-mentioned cast or template is due to by its shape, structure and the subsidiary and impact of the corresponding requirements on filter and system that is that come, and the scope of application is limited.Owing to comparing current filter element (such as organic filter film) on sintering diamond bit filter element is in the repellence, material irreversible membrane fouling repellence, mechanical strength etc. of chemical erosion, there is stronger advantage, therefore, to develop in multiple field can the original filter element of corresponding substitute novel sintered metal polyporous material filter element highly significant.
On above-mentioned background basis, applicant's initiative proposes a kind of flexible, porous metal forming of exploitation.That is, by metal polyporous material form and can bend even foldable thin slice more freely.
Paper " Chinese material is in progress for the progress of Ti-Al intermetallic compound porous material, river Yao etc., the 29th volume, the 3rd phase, in March, 2010 " the 2.3rd in joint describe a kind of preparation technology of Ti-Al intermetallic compound paper mold film.Because above-mentioned paper mold film is made up of Ti-Al intermetallic compound, be therefore still a kind of rigid material.
Summary of the invention
First the present invention will provide the preparation method of several flexible, porous metal forming and flexible, porous metal forming; Its secondary preparation method that several multicellular metal foil (flexible and rigidity) is provided of the present invention; The present invention also will provide the masking frock that can be used for said method.
The first flexible, porous metal forming that the present invention will provide, it is the thin slice that the metal polyporous material being matrix phase by the metal simple-substance of solid solution alloy, face-centred cubic structure or the metal simple-substance of body-centered cubic structure is formed, the thickness of this thin slice is 5 ~ 200 μm, average pore size is 0.05 ~ 100 μm, porosity is 15 ~ 70%, and is formed by the diaphragm sintering of a homogeneous.Specifically, first this flexible, porous metal forming is that the metal being matrix phase by the metal simple-substance of the metal simple-substance of solid solution alloy, face-centred cubic structure or body-centered cubic structure is formed on material composition, thus ensures the flexibility of this flexible, porous metal forming.Secondly, the metal material forming this flexible, porous metal forming should be porous material, and its Pore Characterization is average pore size is 0.05 ~ 100 μm, and porosity is 15 ~ 70%, and like this, flexible, porous metal forming can meet isolated by filtration requirement widely.In addition, the thickness of flexible, porous metal forming (thin slice) is 5 ~ 200 μm, is generally 10 ~ 60 μm.The more important thing is, this flexible, porous metal forming is sintered by the diaphragm of a homogeneous and forms.So-called " homogeneous " represents that the composition of diaphragm is even haply, be namely different from essence mention in background technology " progress of Ti-Al intermetallic compound porous material " have passed through aluminum coated steel after, aluminium foil before Reactive Synthesis.Aluminium foil after aluminum coated steel, before Reactive Synthesis can be regarded as a kind of thin slice of asymmetric form.And the implication of " asymmetric " is general in sintering diamond bit field." homogeneous " in the present invention be namely relative to " asymmetric " propose distinguish concept.Form because flexible, porous metal forming of the present invention is sintered by the diaphragm of a homogeneous, therefore this paillon foil pore-size distribution evenly, paillon foil flatness etc. is better.
The metal polyporous material that described thin slice can be matrix phase by unlimited solid solution alloy is formed.Such as, the metal polyporous material that described thin slice is matrix phase by Ag-Au solid solution, Ti-Zr solid solution, Mg-Cd solid solution or Fe-Cr solid solution is formed.Again such as, described thin slice is preferably made up of Ni-Cu solid solution metal polyporous material, at this moment can require there is more than 75% aperture difference in numerous holes of this porous material in the scope being less than 70 μm.In addition, Ni-Cu solid solution metal polyporous material is all more satisfactory in flexible (can repeatedly folding) and chemical stability etc., and also very excellent in the permeability of the porous material of sintering formation, and therefore range of application is relatively extensive.
The metal polyporous material that described thin slice can also be matrix phase by limit solid solution alloy is formed.Such as, the metal polyporous material that described thin slice is matrix phase by Cu-Al solid solution, Cu-Zn solid solution, Fe-C-Cr solid solution is formed.The metal polyporous material that described thin slice can be also matrix phase by Al, Ni, Cu or Pb of face-centred cubic structure is formed.The metal polyporous material that described thin slice can also be matrix phase by Cr, W, V or Mo of body-centered cubic structure is formed.
Above-mentioned flexible, porous metal forming of the present invention has wide application space, such as: industrially, can be used for the waste heat recovery in weaving and leather industry, medicament reclaims, Environmental capacity, purification in food-processing industry, concentrated, sterilization, byproduct reclaim, medicine and healthcare industry in artificial tracheae, Co ntrolled release, blood filtration, Water warfare, the cleaner in auto industry; The dust-filtering material of mouth mask and the curtain material of static electrification dedusting function is can be used as on civilian.
The step of a kind of preparation method of the present invention's above-mentioned flexible, porous metal forming comprises: the raw meal dispersant and binding agent that form its metal polyporous material are configured to thick suspension by (1); (2) make it to dry the diaphragm of formation one homogeneous in the shaping mold cavity described suspension being injected masking frock; (3) then carry out constraint in the sintering frock of described diaphragm loading and this diaphragm profile being coincide to sinter, take out in sintering frock after sintering and obtain flexible, porous metal forming.
In said method, as the metal polyporous material of flexible, porous metal forming by Ni-Cu solid solution is formed, in order to prepare high performance Ni-Cu flexible, porous metal forming, then, in step (1), first Ni powder and Cu powder are uniformly mixed to form raw meal, wherein Cu opaque amount is 30 ~ 60% of raw meal quality, then be dispersant with ethanol, take PVB as binding agent, be (0.5 ~ 5) in the mass ratio of PVB and ethanol: PVB adds in ethanol by the ratio of 100 makes PVB solution, after this in the ratio adding raw meal 20 ~ 50g in every 100ml ethanol, raw meal is added in PVB solution again, by stirring, raw meal is fully uniformly dispersed, obtain thick suspension, in step (3), sintering process comprises and sintering temperature is risen to 520 ~ 580 DEG C gradually and is incubated the first sintering stage of 60 ~ 180min and after the first stage, is directly warming up to 1130 ~ 1180 DEG C with the heating rate of >=5 DEG C/min and is incubated second sintering stage of 120 ~ 300min.
Can be used for the masking frock of said method, comprising: fixed part, it is framed that described fixed part comprises for shaping diaphragm edge; Adjusting portion, described adjusting portion comprises and the framed template coordinated for shaping diaphragm bottom surface, and described template is connected with the adjusting device that can make the movement on framed depth direction of this template; Movable part, described movable part comprises and is positioned at framed end face and cutting edge and framed end face keep the scraper that flushes in the course of the work.This masking frock can control the thickness of diaphragm more accurately, and ensures the uniformity of diaphragm thickness and the flatness of membrane surface.
As a kind of detailed description of the invention of described adjusting device, adjusting device comprises relative fixing and be connected and the height adjustment mechanism worked alone with corner, template bottom surface respectively with framed.Can regulate the corner height of template respectively like this, ensure the depth of parallelism of formwork integral and framed end face, the thickness of diaphragm is evenly higher.
In addition, the forming surface of described framed forming surface and template is also further provided with volatilizable lubricant coating at 580 DEG C.Wherein, lubricant coating can specifically adopt vaseline coating.Like this, just can ensure that shaping diaphragm takes out from masking frock smoothly, prevents sticking to mould, simultaneously due to the volatile of lubricant coating, the composition of the flexible, porous metal forming of follow-up preparation is not impacted, and is conducive to the porosity improving flexible, porous metal forming on the contrary.
Take out from masking frock smoothly for ease of shaping diaphragm, also can lay PE plastic sheeting or PET film in the forming surface of framed forming surface and template.In shaping mold cavity, add suspension again after forming surface is laid PE plastic sheeting or PET film, after dry formation diaphragm, this diaphragm can not occur bonding with masking frock, and the demoulding is very convenient.
Can be used for the diaphragm sintering frock of said method, comprise the upper die and lower die and limit mould be made up of exotic material, described upper die and lower die coordinate with limit mould respectively thus form the die cavity being used for matching with the diaphragm of inside; Described die cavity is connected with the exhaust structure for distributing sintering volatile matter, and described exhaust structure is the pore set by the fit clearance reserved at the matching part of patrix and limit mould and/or the fit clearance reserved at the matching part of counterdie and limit mould and/or at least one in upper die and lower die and limit mould.Constraint sintering can be carried out to diaphragm by this sintering frock, prevent from being out of shape in the sintering of diaphragm.
As the preferred concrete structure of one of upper die and lower die and limit mould, described limit mould is a mask, and upper die and lower die are respectively clamping plate, is provided with at least triple laminate in described mask, forms described die cavity between two laminated planks of arbitrary neighborhood.This makes it possible to realize multiple diaphragm sinter simultaneously, both enhanced productivity, also can ensure to sinter uniformity simultaneously.
In addition, described upper die and lower die and limit mould are also provided with further for the surface contacted with diaphragm use aluminum oxide coating layer.Aluminium oxide can intercept the element phase counterdiffusion between sintering frock own material with diaphragm material in high-temperature sintering process.
In described upper die and lower die and limit mould, at least one can be made up of graphite.Graphite has good resistance to elevated temperatures, and due to graphite surface smooth, also can be convenient to the demoulding sintering rear product.
The flexible, porous metal forming of the second provided by the present invention is the thin slice that the metal polyporous material being matrix phase by solid solution alloy is formed, and the thickness of this thin slice is 5 ~ 200 μm, average pore size is 0.05 ~ 100 μm, and porosity is 15 ~ 70%.Specifically, this flexible, porous metal forming is that the metal being matrix phase by solid solution alloy is formed on material composition, thus ensures the flexibility of this flexible, porous metal forming.Secondly, the metal material forming this flexible, porous metal forming is porous material, and its Pore Characterization is average pore size is 0.05 ~ 100 μm, and porosity is 15 ~ 70%, and like this, flexible, porous metal forming can meet isolated by filtration requirement widely.In addition, the thickness of flexible, porous metal forming (thin slice) is 5 ~ 200 μm, is generally 10 ~ 60 μm.
The metal polyporous material that described thin slice can be matrix phase by unlimited solid solution alloy is formed.Such as, the metal polyporous material that described thin slice is matrix phase by Ag-Au solid solution, Ti-Zr solid solution, Mg-Cd solid solution or Fe-Cr solid solution is formed.Again such as, described thin slice is preferably made up of Ni-Cu solid solution metal polyporous material, and Ni-Cu solid solution metal polyporous material is all more satisfactory in flexible (can repeatedly folding) and chemical stability etc., and therefore range of application is relatively extensive.
The metal polyporous material that described thin slice can also be matrix phase by limit solid solution alloy is formed.Such as, the metal polyporous material that described thin slice is matrix phase by Cu-Al solid solution, Cu-Zn solid solution, Fe-C-Cr solid solution is formed.
Above-mentioned the second flexible, porous metal forming of the present invention industrially can be used for weave and leather industry in waste heat recovery, medicament recovery, Environmental capacity, purification in food-processing industry, concentrated, sterilization, byproduct reclaim, medicine and healthcare industry in artificial tracheae, Co ntrolled release, blood filtration, Water warfare, the cleaner in auto industry; The dust-filtering material of mouth mask and the curtain material of static electrification dedusting function is can be used as on civilian.
A kind of preparation method's step of the second flexible, porous metal forming of the present invention comprises: (1) prepares carrier, the paillon foil that carrier is made up of a certain element in the metal polyporous material forming flexible, porous metal forming or several element; (2) the raw meal dispersant made by all the other elements forming metal polyporous material and binding agent are configured to thick suspension; (3) described suspension be attached to carrier surface and make it to dry the diaphragm being formed and be attached on carrier surface; (4) sintering then carrying out constraint in the sintering frock that carrier loads and its profile is coincide of attachment diaphragm, taking out in sintering frock after sintering and obtaining flexible, porous metal forming.
Can be used for the masking frock of the preparation method of above-mentioned the second flexible, porous metal forming, it comprises: fixed part, and it is framed that described fixed part comprises for shaping diaphragm edge; Adjusting portion, described adjusting portion comprises and the framed template coordinated for placing carrier, and described template is connected with the adjusting device that can make the movement on framed depth direction of this template; Movable part, described movable part comprises and is positioned at framed end face and cutting edge and framed end face keep the scraper that flushes in the course of the work.This masking frock can control the thickness of diaphragm more accurately, and ensures the uniformity of diaphragm thickness and the flatness of membrane surface.
As a kind of detailed description of the invention of described adjusting device, adjusting device comprises relative fixing and be connected and the height adjustment mechanism worked alone with corner, template bottom surface respectively with framed.Can regulate the corner height of template respectively like this, ensure the depth of parallelism of formwork integral and framed end face, the thickness of diaphragm is evenly higher.
Equally, take out from masking frock smoothly for ease of shaping diaphragm, PE plastic sheeting or PET film can be laid in the forming surface of framed forming surface and template.In shaping mold cavity, add suspension again after forming surface is laid PE plastic sheeting or PET film, after dry formation diaphragm, this diaphragm can not occur bonding with masking frock, and the demoulding is very convenient.
Can be used for the sintering frock of the preparation method of above-mentioned the second flexible, porous metal forming, comprise the upper die and lower die and limit mould be made up of exotic material, described upper die and lower die coordinate with limit mould respectively thus form the die cavity that the carrier for adhering to diaphragm matches; Described die cavity is connected with the exhaust structure for distributing sintering volatile matter, and described exhaust structure is the pore set by the fit clearance reserved at the matching part of patrix and limit mould and/or the fit clearance reserved at the matching part of counterdie and limit mould and/or at least one in upper die and lower die and limit mould.Constraint sintering can be carried out to the carrier of attachment diaphragm by this sintering frock, prevent it to be out of shape in sintering.
As the preferred concrete structure of one of upper die and lower die and limit mould, described limit mould is a mask, and upper die and lower die are respectively clamping plate, is provided with at least triple laminate in described mask, forms described die cavity between two laminated planks of arbitrary neighborhood.Sinter while this makes it possible to realize multiple attachment film carrier, both enhanced productivity, also can ensure to sinter uniformity simultaneously.
In addition, upper die and lower die and limit mould are also provided with further for the surface contacted with diaphragm use aluminum oxide coating layer.Aluminium oxide can intercept sintering frock own material and the element phase counterdiffusion between carrier and diaphragm material in high-temperature sintering process.
In described upper die and lower die and limit mould, at least one is made up of graphite.Graphite has good resistance to elevated temperatures, and due to graphite surface smooth, also can be convenient to the demoulding sintering rear product.
It may be noted that can be identical on the masking frock that the preparation method of above-mentioned the second flexible, porous metal forming uses and the masking frock that sintering frock and the preparation method of the first flexible, porous metal forming above-mentioned use and agglomerant assembling structure.Difference is, need place carrier when the masking frock of second method uses in template, and in template, does not place carrier when the masking frock of first method uses; What place in its die cavity of sintering frock of second method is the carrier (being unsymmetric structure) of attachment diaphragm, and what place in its die cavity of sintering frock of first method is the diaphragm of homogeneous.
The third flexible, porous metal forming of the present invention, it is the thin slice that the metal polyporous material being matrix phase by the metal simple-substance of solid solution alloy, face-centred cubic structure or the metal simple-substance of body-centered cubic structure is formed, the thickness G reatT.GreaT.GT 200 μm of this thin slice and≤1500 μm, average pore size are 0.05 ~ 100 μm, and porosity is 15 ~ 70%.The third flexible, porous metal forming can with the first flexible, porous metal forming above-mentioned preparation method prepare (namely by a homogeneous diaphragm sinter form).When the third flexible, porous metal forming be the metal polyporous material being matrix phase by solid solution alloy form thin slice time, this third flexible, porous metal forming also can be prepared by the preparation method of above-mentioned the second flexible, porous metal forming.
The metal polyporous material that the described thin slice forming the third flexible, porous metal forming can be matrix phase by unlimited solid solution alloy is formed.Such as, the metal polyporous material that described thin slice is matrix phase by Ag-Au solid solution, Ti-Zr solid solution, Mg-Cd solid solution or Fe-Cr solid solution is formed.Again such as, described thin slice is preferably made up of Ni-Cu solid solution metal polyporous material, at this moment can require there is more than 75% aperture difference in numerous holes of this porous material in the scope being less than 70 μm.In addition, Ni-Cu solid solution metal polyporous material is all more satisfactory in flexible (can repeatedly folding) and chemical stability etc., and also very excellent in the permeability of the porous material of sintering formation, and therefore range of application is relatively extensive.
The metal polyporous material that the thin slice forming the third flexible, porous metal forming can also be matrix phase by limit solid solution alloy is formed.Such as, the metal polyporous material that described thin slice is matrix phase by Cu-Al solid solution, Cu-Zn solid solution, Fe-C-Cr solid solution is formed.The metal polyporous material that this thin slice can be also matrix phase by Al, Ni, Cu or Pb of face-centred cubic structure is formed.The metal polyporous material that described thin slice can also be matrix phase by Cr, W, V or Mo of body-centered cubic structure is formed.
Compared to the first flexible, porous metal forming above-mentioned and the second flexible, porous metal forming, the thickness of the third flexible, porous metal forming is thicker, therefore, the intensity of the third flexible, porous metal forming can higher than the intensity of the first flexible, porous metal forming and the second flexible, porous metal forming, therefore in application, the third flexible, porous metal forming is more suitable for the occasion higher to its intensity.A typical example application the third flexible, porous metal forming is made into the filter bag filtered.Filter bag is widely used in filter bag type deduster, but the bag of existing filter bag is many is made into by organic fiber, therefore also referred to as " cloth bag ", it exists the shortcomings such as high temperature resistant property difference, filtering accuracy are not high.The present invention will provide a kind of filter bag filtered, it comprises bag, described bag is made up of the third flexible, porous metal forming above-mentioned, the third flexible, porous metal forming is not easily damaged because of factors such as frequent blowbacks in filter bag use procedure faster because there being higher intensity, simultaneously has good high temperature resistant property due to its material behavior.
Except the preparation method of the above-mentioned flexible, porous metal forming provided, present invention also offers the preparation method of the multicellular metal foil of following several improvement, both can be used for preparing above-mentioned flexible, porous metal forming, and also can be used for the multicellular metal foil preparing other.A kind of preparation method improving multicellular metal foil, this multicellular metal foil is the thin slice be made up of metal polyporous material, and its step comprises: the raw meal dispersant and binding agent that form its metal polyporous material are configured to thick suspension by (1); (2) the dry diaphragm forming a homogeneous is made it in the shaping mold cavity described suspension being injected masking frock; (3) compacting is carried out to diaphragm and improve Powder Particles Packing density in diaphragm; (4) multicellular metal foil is obtained after being sintered by compacting rear film.The method may be used for preparing the first flexible, porous metal forming above-mentioned, the second flexible, porous metal forming and the third flexible, porous metal forming.Because the compacting (can adopt the compactings such as roll mill, moulding press, isostatic pressing machine) of its step (3) improves Powder Particles Packing density in diaphragm, the average pore size of flexible, porous metal forming can be made less and evenly; By can control the mean pore size of flexible, porous metal forming to the selection of pressing pressure.
The preparation method of the another kind of multicellular metal foil improved, this multicellular metal foil is the thin slice be made up of metal polyporous material, and its step comprises: the raw meal dispersant and binding agent that form its metal polyporous material are configured to pureed lotion by (1); (2) carry out suppressing the diaphragm forming homogeneous to lotion; (3) multicellular metal foil is obtained after being sintered by compacting rear film.The method may be used for preparing the first flexible, porous metal forming above-mentioned, the second flexible, porous metal forming and the third flexible, porous metal forming.Because the compacting (can adopt the compactings such as roll mill, moulding press, isostatic pressing machine) of its step (2) improves Powder Particles Packing density in diaphragm, the average pore size of flexible, porous metal forming can be made less and evenly; By can control the mean pore size of flexible, porous metal forming to the selection of pressing pressure.
The preparation method of another multicellular metal foil improved, this multicellular metal foil is the thin slice be made up of metal polyporous material, its step comprises: (1) prepares carrier, and described carrier is the paillon foil be made up of a certain element in the metal polyporous material forming flexible, porous metal forming or several element; (2) the raw meal dispersant made by all the other elements forming metal polyporous material and binding agent are configured to thick suspension; (3) described suspension be attached to carrier surface and make it dry and form the diaphragm be attached on carrier surface; (4) compacting is carried out to the carrier of attachment diaphragm and improve Powder Particles Packing density in diaphragm; (5) after sintering, multicellular metal foil is obtained to the carrier of attachment diaphragm after compacting.The method may be used for preparing above-mentioned the second flexible, porous metal forming and the third flexible, porous metal forming.Because the compacting (can adopt the compactings such as roll mill, moulding press, isostatic pressing machine) of its step (4) improves Powder Particles Packing density in diaphragm, the average pore size of flexible, porous metal forming can be made less and evenly; By flexible, porous metal forming mean pore size can be controlled to the selection of pressing pressure.
Need point out, the preparation method of the multicellular metal foil of this several improvement above-mentioned can use above-mentioned masking frock and sintering frock equally.In addition, in the preparation method of the flexible, porous metal forming of above-mentioned several improvement, the pressure used during its compacting can be 5 ~ 300MPa, is generally 10 ~ 100MPa.Generally speaking, during compacting, pressure is larger, and the average pore size of multicellular metal foil is less and more even, and the globality of multicellular metal foil and intensity are also higher, but porosity is less.
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.The aspect that the present invention adds and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Fig. 1 is the appearance schematic diagram of a kind of rectangular flexible multicellular metal foil in the specific embodiment of the invention.
Fig. 2 is for preparing the perspective view of the masking frock of the flexible, porous metal forming shown in Fig. 1.
Fig. 3 be in Fig. 2 I-I to sectional view.
Fig. 4 is for preparing the structural representation of the diaphragm sintering frock of the flexible, porous metal forming shown in Fig. 1.
Fig. 5 be in Fig. 4 II-II to sectional view.
Detailed description of the invention
A kind of flexible, porous metal forming 100 as shown in Figure 1, it is the thin slice that the metal polyporous material being matrix phase by the metal simple-substance of solid solution alloy, face-centred cubic structure or the metal simple-substance of body-centered cubic structure is formed, the thickness H of this thin slice is 5 ~ 1500 μm, average pore size is 0.05 ~ 100 μm, and porosity is 15 ~ 70%.Wherein, the shape of thin slice can be the rectangle shown in Fig. 1, also can be other flat shapes such as circular, oval.
The step of a kind of preparation method (method 1) of above-mentioned flexible, porous metal forming 100 comprises: the raw meal dispersant and binding agent that form its metal polyporous material are configured to thick suspension by (1); (2) make it to dry the diaphragm of formation one homogeneous in the shaping mold cavity described suspension being injected masking frock; (3) then carry out constraint in the sintering frock of described diaphragm loading and this diaphragm profile being coincide to sinter, take out in sintering frock after sintering and obtain flexible, porous metal forming 100.
In said method, dispersant can use the surface tension such as ethanol, MEK, toluene little and the fast easily dry organic solvent of volatilization; Binding agent can use PVB, PVA, PVC, polyvinyl alcohol, polyethylene glycol (low-molecular-weight wax class), paraffin, fatty acid, aliphatic amide type and ester class etc.
In said method, the ratio between raw meal and dispersant can according to the concrete composition of raw meal to ensure that the surface quality of drying rear film is determined for principle.Generally speaking, if the too high levels of raw meal, then the surface quality of drying rear film is bad, easily occurs the phenomenons such as be full of cracks; If the content of raw meal is too low, then can increases the follow-up number of times described suspension being injected masking frock shaping mold cavity, extend the manufacturing cycle of flexible, porous metal forming.
In said method, the ratio between binding agent and dispersant can be determined to ensure to dry the surface quality of rear film and membrane ruggedness for principle according to the concrete composition of raw meal.Generally speaking, if binder content is too high, then suspension poor fluidity, easily has the defects such as shrinkage cavity after oven dry, and demoulding difficulty after sintering; If binder content is too low, can not be effectively bonding between the powder particle of raw meal, diaphragm insufficient formability, membrane ruggedness are low and taking-up is difficult.
In said method, constraint sintering sinters under referring to and keeping the prerequisite of diaphragm shapes by sintering frock, prevents diaphragm from deforming in sintering process.Concrete sintering schedule should be determined according to the concrete composition of raw meal and the pore structure that will reach.
As the improvement to said method, also can increase a step in its step (2) and step (3), namely compacting be carried out to diaphragm and improve Powder Particles Packing density in diaphragm, and then sinter.Wherein specifically can adopt the compactings such as roll mill, moulding press, isostatic pressing machine.Compacting can improve Powder Particles Packing density in diaphragm, make the average pore size of the flexible, porous metal forming of final preparation less and evenly; By flexible, porous metal forming mean pore size can be controlled to the selection of pressing pressure.
Masking frock as shown in figures 2-3 will be used in the step 2 of said method.Specifically, this masking frock comprises fixed part 210, described fixed part 210 comprises for shaping diaphragm edge framed 211, and this framed 211 is arranged on a base for supporting 212 to support (certainly framed 211 also can be fixed by other modes) framed 211; Adjusting portion 220, described adjusting portion 220 comprises the template 221 coordinated with framed 211 for shaping diaphragm bottom surface, and described template 221 is connected with the adjusting device 222 that can make the movement on the depth direction of framed 211 of this template 221; And movable part 230, described movable part 230 comprises and is positioned at framed 211 end faces and cutting edge and framed 211 end faces keep the scraper 231 that flushes in the course of the work.When the shape of flexible, porous metal forming 100 is the rectangles shown in Fig. 1, the inner chamber of framed 211 is also a rectangle, and template 221 is positioned at this inner chamber and coordinates with rectangular inner cavity.In addition, adjusting device 222 specifically can comprise 211 relative fixing and be connected with corner, template 221 bottom surface respectively and the height adjustment mechanism 222a worked alone (such as laying respectively at spiral lifting mechanism below corner, template 221 bottom surface) with framed.For ease of the installation of height adjustment mechanism 222a, the bottom of framed 211 is also provided with the supporting construction 211a extended internally, and described height adjustment mechanism 222a is arranged on supporting construction 211a.
The using method of above-mentioned masking frock is: first by the height that regulates each height adjustment mechanism 222a template 221 to be adjusted to setting and with framed 211 end face keeping parallelisms, and then framed 211 forming surface and template 221 forming surface on lay one deck PET film respectively, then the suspension that step (1) obtains is injected in the shaping mold cavity be made up of framed 211 and template 221, after this movable scraper 231 ensure that its cutting edge flushes with framed 211 end faces when mobile, thus with scraper 231 suspension being attached to more than framed 211 end faces scraped from, again suspension is dried, after drying, suspension is frozen into the uniform diaphragm of thickness, finally diaphragm is taken off from masking frock.Above-mentioned masking frock can control the thickness of diaphragm accurately, and ensures the uniformity of diaphragm thickness and the flatness of membrane surface.
The diaphragm sintering frock will used as shown in Figures 4 and 5 in the step 3 of said method.Specifically, this diaphragm sintering frock comprises patrix 310a, counterdie 310b and the limit mould 320 be made up of graphite, and described patrix 310a, counterdie 310b coordinate with limit mould 320 respectively thus form the die cavity for matching with the diaphragm 100 ' of inside; Wherein, limit mould 320 is specially a mask 321, and patrix 310a and counterdie 310b is respectively clamping plate 310, is provided with multiply-plywood 310 in described mask 321, forms described die cavity between two laminated planks 310 of arbitrary neighborhood; In addition, each clamping plate 310 are also reserved with for distributing the fit clearance sintering volatile matter with the matching part of mask 321.When the shape of flexible, porous metal forming 100 is the rectangles shown in Fig. 1, the sidepiece of described mask 321 is the rectangular configuration be made up of header board 321a, rear plate 321b, left plate 321c and right panel 321d.
The using method of above-mentioned diaphragm sintering frock is: first on the inwall of mask 321 and the two side of each clamping plate 310, arrange one deck aluminum oxide coating layer (first can use ethanol, PVB and alumina powder are mixedly configured into the alumina powder suspension solution of thickness, then change aluminium powder suspension is coated on the inwall of mask 321 and the two side of each clamping plate 310 and forms aluminum oxide coating layer), then bottom clamping plate 310 are laid in the bottom of mask 321, a diaphragm 100 ' is placed above these clamping plate 310, second layer clamping plate 310 are laid again in the top of this diaphragm 100 ', the like can lay whole clamping plate 310, and ensure respectively to accompany one piece of diaphragm 100 ' between two laminated planks 310 of arbitrary neighborhood, after this diaphragm assembled sintering frock is sent in sintering furnace and sinter, from diaphragm sintering frock, flexible, porous metal forming 100 is taken out after sintering.Therefore, above-mentioned diaphragm sintering frock achieves multiple diaphragm 100 ' and retrains sintering simultaneously, both enhances productivity, and also can ensure to sinter uniformity simultaneously.
The step of the another kind of preparation method (method 2) of above-mentioned flexible, porous metal forming comprises: (1) prepares carrier, and described carrier is the paillon foil be made up of a certain element in the metal polyporous material forming flexible, porous metal forming or several element; (2) the raw meal dispersant made by all the other elements forming metal polyporous material and binding agent are configured to thick suspension; (3) described suspension be attached to carrier surface and make it to dry the diaphragm being formed and be attached on carrier surface; (4) sintering then carrying out constraint in the sintering frock that carrier loads and its profile is coincide of attachment diaphragm, taking out in sintering frock after sintering and obtaining flexible, porous metal forming.As the improvement to the method, a step can be increased in its step (3) and step (4) equally, namely compacting be carried out to the carrier of attachment diaphragm and improve Powder Particles Packing density in diaphragm, and then sinter.Wherein specifically can adopt the compactings such as roll mill, moulding press, isostatic pressing machine.Compacting can improve Powder Particles Packing density in diaphragm, make the average pore size of the flexible, porous metal forming of final preparation less and evenly; By flexible, porous metal forming mean pore size can be controlled to the selection of pressing pressure.
In said method, dispersant can use the surface tension such as ethanol, MEK, toluene little and the fast easily dry organic solvent of volatilization; Binding agent can use PVB, PVA, PVC, polyvinyl alcohol, polyethylene glycol (low-molecular-weight wax class), paraffin, fatty acid, aliphatic amide type and ester class etc.
In said method, the ratio between raw meal and dispersant can according to the concrete composition of raw meal to ensure that the surface quality of drying rear film is determined for principle.Generally speaking, if the too high levels of raw meal, then the surface quality of drying rear film is bad, easily occurs the phenomenons such as be full of cracks; If the content of raw meal is too low, then can increases the follow-up number of times described suspension being injected masking frock shaping mold cavity, extend the manufacturing cycle of flexible, porous metal forming.
In said method, the ratio between binding agent and dispersant can be determined to ensure to dry the surface quality of rear film and membrane ruggedness for principle according to the concrete composition of raw meal.Generally speaking, if binder content is too high, then suspension poor fluidity, easily has the defects such as shrinkage cavity after oven dry, and demoulding difficulty after sintering; If binder content is too low, can not be effectively bonding between the powder particle of raw meal, diaphragm insufficient formability, membrane ruggedness are low and taking-up is difficult.
In said method, constraint sintering sinters under referring to and keeping the prerequisite of diaphragm shapes by sintering frock, prevents diaphragm from deforming in sintering process.Concrete sintering schedule should be determined according to the concrete composition of raw meal and the pore structure that will reach.Diaphragm sintering frock during the method still uses " method 1 ".
The modes such as spraying can be adopted in the step 3 of said method to be attached to carrier surface, but suggestion use the masking frock shown in above-mentioned Fig. 2 ~ 3 that described suspension is attached to carrier surface.Concrete grammar is: first by the height that regulates each height adjustment mechanism 222a template 221 to be adjusted to setting and with framed 211 end face keeping parallelisms, and then carrier is placed in template 221, and the suspension that step (2) obtains is injected into by the shaping mold cavity between framed 211 and carrier, after this movable scraper 231 ensure that its cutting edge flushes with framed 211 end faces when mobile, thus with scraper 231 suspension being attached to more than framed 211 end faces scraped from, again suspension is dried, after drying, suspension is frozen into the uniform diaphragm of thickness, finally the carrier of attachment diaphragm is taken off from masking frock.
The step of another preparation method (method 3) of above-mentioned flexible, porous metal forming comprising: the raw meal dispersant and binding agent that form its metal polyporous material are configured to pureed lotion by (1); (2) carry out suppressing the diaphragm forming homogeneous to lotion; (3) flexible, porous metal forming is obtained after being sintered by compacting rear film.In the method, dispersant can use the surface tension such as ethanol, MEK, toluene little and the fast easily dry organic solvent of volatilization; Binding agent can use PVB, PVA, PVC, polyvinyl alcohol, polyethylene glycol (low-molecular-weight wax class), paraffin, fatty acid, aliphatic amide type and ester class etc.Above-mentioned " method 3 " processing step compares " method 1 " and " method 2 " is less, and production efficiency is high, and the quality of the flexible, porous metal forming prepared is also very desirable.Wherein specifically can adopt the compactings such as roll mill, moulding press, isostatic pressing machine.Compacting can improve Powder Particles Packing density in diaphragm, make the average pore size of the flexible, porous metal forming of final preparation less and evenly; By flexible, porous metal forming mean pore size can be controlled to the selection of pressing pressure.Diaphragm sintering frock during the method uses equally " method 1 ".
Embodiment 1
Flexible, porous metal forming 100 is the rectangular tab be made up of Ni-Cu solid solution alloy porous material, and this sheet thickness H is 10 μm, and length is 160mm, and width is 125mm, and average pore size is 18.4 μm, and porosity is 58.37%.The preparation method of this flexible, porous metal forming 100 is: first, Ni powder and Cu powder are uniformly mixed to form raw meal, wherein Cu opaque amount is 30% of raw meal quality, then be dispersant with ethanol, take PVB as binding agent, be that PVB to add in ethanol and makes PVB solution by the ratio of 2.5:100 in the mass ratio of PVB and ethanol, after this in the ratio adding raw meal 25g in every 100ml ethanol, raw meal is added in PVB solution again, by stirring, raw meal being fully uniformly dispersed, obtaining thick suspension, secondly, make it to dry the diaphragm 100 ' of formation one homogeneous in the shaping mold cavity described suspension being injected masking frock as shown in figures 2-3, then, described diaphragm 100 ' is loaded diaphragm sintering frock as shown in Figures 4 and 5, concrete sintering process first sintering temperature is risen to 550 DEG C gradually and is incubated 90min (Main Function of this process is to remove binding agent, vaseline etc.), then being directly warming up to 1130 DEG C with the heating rate of 6 DEG C/min and being incubated 180min (is rapidly heated to 1170 DEG C of fusing points more than Cu, the mobility after Cu melting can be utilized to drive Ni powder, Ni powder is fully combined, ensure the integrality after flexible, porous metal forming 100 sintering and flexibility), take out in sintering frock after sintering and obtain flexible, porous metal forming 100.
Embodiment 2
Flexible, porous metal forming 100 is the rectangular tab be made up of Ni-Cu solid solution alloy porous material, and this sheet thickness H is 100 μm, and length is 200mm, and width is 130mm, and average pore size is 30 μm, and porosity is 61.68%.The preparation method of this flexible, porous metal forming 100 is: first, Ni powder and Cu powder are uniformly mixed to form raw meal, wherein Cu opaque amount is 60% of raw meal quality, then be dispersant with ethanol, take PVB as binding agent, be that PVB to add in ethanol and makes PVB solution by the ratio of 4:100 in the mass ratio of PVB and ethanol, after this in the ratio adding raw meal 40g in every 100ml ethanol, raw meal is added in PVB solution again, by stirring, raw meal being fully uniformly dispersed, obtaining thick suspension; Secondly, make it to dry the diaphragm 100 ' of formation one homogeneous in the shaping mold cavity described suspension being injected masking frock as shown in figures 2-3; Then, described diaphragm 100 ' is loaded diaphragm sintering frock as shown in Figures 4 and 5, concrete sintering process first sintering temperature is risen to 550 DEG C gradually and is incubated 90min, then be directly warming up to 1180 DEG C with the heating rate of 8 DEG C/min and be incubated 180min, take out in sintering frock after sintering and obtain flexible, porous metal forming 100.
Embodiment 3
Flexible, porous metal forming is the rectangular tab be made up of Ni-Cu solid solution alloy porous material, and this sheet thickness H is 60 μm, and length is 150mm, and width is 100mm, and average pore size is 54.1 μm, and porosity is 40.16%.This flexible, porous metal forming preparation method is: first, be more than 99% to purity, thickness is that the Cu paper tinsel (carrier) of 10 μm carries out surface treatment: adopt mass concentration to be the impurity such as the greasy dirt on the NaOH solution cleaning Cu paper tinsel surface of 10%, Cu paper tinsel is put into the H of mass concentration 10% after washing again
2sO
4pickling two minutes in solution, the oxide on removing Cu paper tinsel surface and rust stain; Again the Cu paper tinsel after alkali cleaning, pickling is immersed in acetone soln and use Ultrasonic Cleaning 8min, finally put into vacuum drying oven and dry, and record Cu paper tinsel quality; Then, with simple substance Ni powder for raw material, be dispersant with ethanol, take PVB as binding agent, be that PVB to add in ethanol and makes PVB solution by the ratio of 4:100 in the mass ratio of PVB and ethanol, after this add in PVB solution in the ratio adding Ni powder 25g in every 100ml ethanol again, by stirring, Ni powder being fully uniformly dispersed, obtaining thick suspension; After this, Cu paper tinsel is close to template 221 surface of masking frock, by the thickness of the Altitude control overlay film of adjustment template 221 end face, then described suspension is injected in the shaping mold cavity of masking frock, Ni and Cu mass ratio is guaranteed to control at about 1:1, then carry out drying and the diaphragm that the blank after drying loads as shown in Figures 4 and 5 is sintered frock, the sintering process identical by embodiment 1 sinters.
Embodiment 4
Flexible, porous metal forming 100 is the rectangular tab be made up of Ni-Cu solid solution alloy porous material, and this sheet thickness H is 10 μm, and length is 160mm, and width is 125mm, and average pore size is 1.2 μm, and porosity is 42.5%.The preparation method of this flexible, porous metal forming 100 is: first, Ni powder and Cu powder are uniformly mixed to form raw meal, wherein Cu opaque amount is 30% of raw meal quality, then be dispersant with ethanol, take PVB as binding agent, be that PVB to add in ethanol and makes PVB solution by the ratio of 2.5:100 in the mass ratio of PVB and ethanol, after this in the ratio adding raw meal 25g in every 100ml ethanol, raw meal is added in PVB solution again, by stirring, raw meal being fully uniformly dispersed, obtaining thick suspension, secondly, make it to dry the diaphragm 100 ' of formation one homogeneous in the shaping mold cavity described suspension being injected masking frock as shown in figures 2-3, then diaphragm 100 ' is put on roll mill and be rolled with the mill speed of 600r/min (roll rotational speed) under 10MPa, then, diaphragm 100 ' after rolling is loaded diaphragm sintering frock as shown in Figures 4 and 5, concrete sintering process first sintering temperature is risen to 550 DEG C gradually and is incubated 90min (Main Function of this process is to remove binding agent, vaseline etc.), then being directly warming up to 1130 DEG C with the heating rate of 6 DEG C/min and being incubated 180min (is rapidly heated to 1170 DEG C of fusing points more than Cu, the mobility after Cu melting can be utilized to drive Ni powder, Ni powder is fully combined, ensure the integrality after flexible, porous metal forming 100 sintering and flexibility), take out in sintering frock after sintering and obtain flexible, porous metal forming 100.
Embodiment 5
Flexible, porous metal forming is the rectangular tab be made up of Ni-Cu solid solution alloy porous material, and this sheet thickness H is 60 μm, and length is 150mm, and width is 100mm, and average pore size is 25 μm, and porosity is 37%.This flexible, porous metal forming preparation method is: first, be more than 99% to purity, thickness is that the Cu paper tinsel (carrier) of 10 μm carries out surface treatment: adopt mass concentration to be the impurity such as the greasy dirt on the NaOH solution cleaning Cu paper tinsel surface of 10%, Cu paper tinsel is put into the H of mass concentration 10% after washing again
2sO
4pickling two minutes in solution, the oxide on removing Cu paper tinsel surface and rust stain; Again the Cu paper tinsel after alkali cleaning, pickling is immersed in acetone soln and use Ultrasonic Cleaning 8min, finally put into vacuum drying oven and dry, and record Cu paper tinsel quality; Then, with simple substance Ni powder for raw material, be dispersant with ethanol, take PVB as binding agent, be that PVB to add in ethanol and makes PVB solution by the ratio of 4:100 in the mass ratio of PVB and ethanol, after this add in PVB solution in the ratio adding Ni powder 25g in every 100ml ethanol again, by stirring, Ni powder being fully uniformly dispersed, obtaining thick suspension; After this, Cu paper tinsel is close to template 221 surface of masking frock, by the thickness of the Altitude control overlay film of adjustment template 221 end face, then described suspension is injected in the shaping mold cavity of masking frock, Ni and Cu mass ratio is guaranteed to control at about 1:1, then carry out drying and the blank after oven dry is put on machine and be rolled with the mill speed of 300r/min (roll rotational speed) under 15MPa, then load diaphragm sintering frock as shown in Figures 4 and 5, the sintering process identical by embodiment 1 sinters.
Embodiment 6
Flexible, porous metal forming 100 is the rectangular tab be made up of Ni-Cu solid solution alloy porous material, and this sheet thickness H is 500 μm, and length is 160mm, and width is 125mm, and average pore size is 15.2 μm, and porosity is 51%.The preparation method of this flexible, porous metal forming 100 is: first, Ni powder and Cu powder are uniformly mixed to form raw meal, wherein Cu opaque amount is 30% of raw meal quality, then be dispersant with ethanol, take PVB as binding agent, become pureed lotion by the proportional arrangement of every 100ml ethanolic solution 30gPVB, 500g raw meal; Secondly, lotion is put on roll mill and be rolled with the mill speed of 200r/min (roll rotational speed) under 25MPa; Then, diaphragm 100 ' after rolling is loaded diaphragm sintering frock as shown in Figures 4 and 5, concrete sintering process first sintering temperature is risen to 550 DEG C gradually and is incubated 90min, then being directly warming up to 1130 DEG C with the heating rate of 6 DEG C/min and being incubated 180min (is rapidly heated to 1170 DEG C of fusing points more than Cu, the mobility after Cu melting can be utilized to drive Ni powder, Ni powder is fully combined, ensure the integrality after flexible, porous metal forming 100 sintering and flexibility), take out in sintering frock after sintering and obtain flexible, porous metal forming 100.
Embodiment 7
Embodiment 7 is on the basis of embodiment 1, and sheet thickness being increased to H is 300 μm.
Embodiment 8
Embodiment 8 is on the basis of embodiment 4, and sheet thickness being increased to H is 500 μm.
Embodiment 9
Embodiment 9 is on the basis of embodiment 5, and sheet thickness being increased to H is 800 μm.
The flexible, porous metal forming performance comparison result of embodiment 1 ~ 9 is as shown in table 1.
Table 1: flexible, porous metal forming performance comparison result
Claims (10)
1. the preparation method of multicellular metal foil, this multicellular metal foil is the thin slice be made up of metal polyporous material, and its step comprises: the raw meal dispersant and binding agent that form its metal polyporous material are configured to thick suspension by (1); (2) the dry diaphragm forming a homogeneous is made it in the shaping mold cavity described suspension being injected masking frock; (3) compacting is carried out to diaphragm and improve Powder Particles Packing density in diaphragm; (4) flexible, porous metal forming is obtained after being sintered by compacting rear film.
2. the preparation method of multicellular metal foil, this multicellular metal foil is the thin slice be made up of metal polyporous material, and its step comprises: the raw meal dispersant and binding agent that form its metal polyporous material are configured to pureed lotion by (1); (2) carry out suppressing the diaphragm forming homogeneous to lotion; (3) flexible, porous metal forming is obtained after being sintered by compacting rear film.
3. the preparation method of multicellular metal foil, this multicellular metal foil is the thin slice be made up of metal polyporous material, its step comprises: (1) prepares carrier, and described carrier is the paillon foil be made up of a certain element in the metal polyporous material forming flexible, porous metal forming or several element; (2) the raw meal dispersant made by all the other elements forming metal polyporous material and binding agent are configured to thick suspension; (3) described suspension be attached to carrier surface and make it dry and form the diaphragm be attached on carrier surface; (4) compacting is carried out to the carrier of attachment diaphragm and improve Powder Particles Packing density in diaphragm; (5) after sintering, flexible, porous metal forming is obtained to the carrier of attachment diaphragm after compacting.
4. as the method in claims 1 to 3 as described in any one claim, it is characterized in that: described multicellular metal foil is flexible, porous metal forming, the thin slice that the metal polyporous material that this flexible, porous metal forming is matrix phase by the metal simple-substance of solid solution alloy, face-centred cubic structure or the metal simple-substance of body-centered cubic structure is formed, the thickness of this thin slice is 5 ~ 1500 μm, average pore size is 0.05 ~ 100 μm, and porosity is 15 ~ 70%.
5. method as claimed in claim 4, is characterized in that: the metal polyporous material that described thin slice is matrix phase by unlimited solid solution alloy is formed.
6. method as claimed in claim 5, is characterized in that: the metal polyporous material that described thin slice is matrix phase by Ag-Au solid solution, Ti-Zr solid solution, Mg-Cd solid solution, Fe-Cr solid solution or Ni-Cu solid solution is formed.
7. method as claimed in claim 4, is characterized in that: the metal polyporous material that described thin slice is matrix phase by limit solid solution alloy is formed.
8. method as claimed in claim 7, is characterized in that: the metal polyporous material that described thin slice is matrix phase by Cu-Al solid solution, Cu-Zn solid solution, Fe-C-Cr solid solution is formed.
9. method as claimed in claim 4, is characterized in that: the metal polyporous material that described thin slice is matrix phase by Al, Ni, Cu or Pb of face-centred cubic structure is formed.
10. method as claimed in claim 4, is characterized in that: the metal polyporous material that described thin slice is matrix phase by Cr, W, V or Mo of body-centered cubic structure is formed.
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