CN110330339A - A kind of large scale MAX phase ceramics impeller preparation method - Google Patents

A kind of large scale MAX phase ceramics impeller preparation method Download PDF

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CN110330339A
CN110330339A CN201910605087.8A CN201910605087A CN110330339A CN 110330339 A CN110330339 A CN 110330339A CN 201910605087 A CN201910605087 A CN 201910605087A CN 110330339 A CN110330339 A CN 110330339A
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impeller
max phase
large scale
slurry
phase ceramics
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CN110330339B (en
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燕青芝
赵占冲
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University of Science and Technology Beijing USTB
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Abstract

The present invention provides a kind of preparation method of large scale MAX phase ceramics impeller, this method can prepare the MAX phase ceramics impeller with large scale, complicated shape feature.Using gel casting technique, introduces argon gas and richness A atmosphere does sintering protective atmosphere, no pressing phase sintering MAX phase ceramics impeller.Preparation method technical process includes, and prepares ceramic slurry, injection molding, demoulding, drying, green machined, degumming, pressureless sintering, polishing refine.The present invention solves that MAX phase ceramics slurry density is easily settled greatly, and the technical problems such as easy to crack, deformation in dry and sintering process finally realize the successful preparation of large scale MAX phase ceramics impeller.The impeller has the superperformances such as corrosion-resistant, radiation resistance, wear-resistant, resistance to oxidation, high temperature resistant, can be widely applied to the industries such as nuclear power, chemical industry, metallurgy, oil field, mine, thermoelectricity.

Description

A kind of large scale MAX phase ceramics impeller preparation method
Technical field
The present invention is a kind of large scale MAX phase ceramics impeller preparation method, belongs to technical field of material, and in particular to one The preparation method that the pressureless sintering based on gel casting forming prepares MAX phase ceramics impeller is planted, made impeller has large scale, answers Miscellaneous shape and corrosion-resistant, radiation resistance, wear-resistant, resistance to oxidation, technical characteristic resistant to high temperature.
Background technique
Centrifugal pump is the indispensable equipment of the industries trandfer fluid such as nuclear energy, chemical industry, metallurgy, oil field, mine, thermoelectricity, and Impeller is the core flow passage components of centrifugal pump conveying liquid.In order to reliably pump the spies such as high temperature, high irradiation, high corrosion, high abrasion Different fluid needs impeller that can bear irradiation, burn into abrasion, high temperature and complex stress for a long time.Common impeller material is for example stainless Steel, ultra high molecular polyethylene, fluoroplastics, hard alloy, acrylonitrile-butadiene rubber etc. can not be long-term reliable in above-mentioned environment It is on active service, application is restricted.A kind of impeller of pump material for being able to satisfy above-mentioned Service Environment and requiring is explored, above-mentioned industry is become The problem of developing urgent need to resolve.
MAX phase is a kind of processable advanced ceramics that can be conductive of stratiform, and MAX phase combines ceramic material and metal material Lot of advantages, these advantages derive from the unique stacked structure of the covalent M-X key of strong metal and weak interatomic M-A key.Therefore, MAX phase ceramics show high creep resistance under low-density, low heat expansion, low-friction coefficient, high temperature, high rigidity, high intensity, High-modulus, good conduction/heating conduction, thermal shock resistance, antibody Monoclonal tolerance and excellent high temperature oxidation resistance etc..This A series of excellent performances make it have wide application prospect, also therefore cause the extensive concern of researcher.MAX phase ceramics It is assessed as the candidate material of the centrifugal pump impeller suitable for certain complicated harsh Service Environments at present.Regrettably, this tool Having large scale, complicated shape and the MAX phase impeller being on active service in extremely complicated harsh environment, there are no pertinent literature reports.
Gel injection-moulding is a kind of method of novel near-net-shape ceramic material, is to traditional ceramics and polymerization Learn the integrated application of concept.The organic monomer solution of the technology utilization hybrid ceramic powder is handed under initiator and catalyst action Connection aggregates into three-dimensional network polymer gel, so that the green body of consolidation in-situ forming complexity and uniform microstructure, is mainly used for The molding of large scale, complicated shape ceramic part has green compact compared with powder metallurgy forming and common dry powder compression moulding The advantages that intensity height, even density.Therefore gel injection-moulding is the ideal preparation side of large scale, complicated shape MAX phase ceramics impeller Method.
Article " the Synthesis of nanolayered Ti of foreign scholar Foratirad3SiC2MAX phase via Infiltration of porous TiC preform produced by the gelcasting process " is reported Using Gel-casting process forming porous TiC ceramics, then reaction-sintered prepares bulk Ti3SiC2Ceramics.But with this side The Ti of method preparation3SiC2Ceramics influence the mechanical behavior under high temperature and resistance to LBE corrosivity of material containing a large amount of unreacted free silicas Can, it cannot act as nuclear power reactor coolant circulation impeller of pump.Article " the Textured Ti of Mrinalini3SiC2by Gelcasting in a strong magnetic field " report preparation is prepared for Ti using Gel-casting process3SiC2It is raw Base, still, ceramic green are not able to satisfy the requirement of structural material, cannot act as impeller of pump without sintering, mechanical property Material.Article " the Deflocculation and stabilization of Ti of A.Idzkowska3SiC2ceramic The green compact that powder in gelcasting process " uses Gel-casting process to be prepared for bending strength as 1.5MPa, but It is that this intensity is not able to satisfy the requirement of impeller of pump material equally.The paper that scholar Hu Chunfeng is delivered " Microstructure and Mechanical Properties of Gel Casted Ti3AlC2 " reports Ti3AlC2 The gel casting of ceramics, still, Ti3AlC2Sample surface layer is decomposed, and resistance to LBE corrosive nature is caused to reduce, meanwhile, consistency It is relatively low that mechanical property is caused to reduce, it is not able to satisfy requirement of the nuclear power heap LBE coolant pump impeller to material property.Foreign scholar Paper " the Ti that M.Potoczek is delivered2AlC foams produced by gel-casting " reports Ti2AlC foamed ceramics Gel casting, still, Ti2AlC foamed ceramics greatly reduces because internal contain a large amount of bubbles as structural material Impeller of pump mechanical property, be not able to satisfy requirement of the nuclear power heap LBE coolant pump impeller to material property.Chinese patent (CN The method for preparing SiC porcelain impeller 102875150B) is taught, still, MAX phase ceramics adhere to different material bodies separately from silicon carbide System, all too many levels of preparation section, for example, gel rubber system selects, and slurry configuration, pouring procedure, drying means, sintering method Etc., all there is the difference of essence,
The present invention uses gel injection molding and forming technology, introduces argon gas and richness A atmosphere does sintering protective atmosphere, no pressing is mutually burnt Knot preparation large scale, complicated shape MAX phase ceramics impeller.
Summary of the invention
The present invention uses gel casting forming, the process without pressing phase sintering, prepares a kind of nuclear power reactor coolant and follows Ring pump MAX phase ceramics impeller, solves many technical problems in preparation flow, realizes large scale, complicated shape, without pressure The successful preparation of the MAX phase ceramics impeller of rich A sintering.Refer to that sintering processing is pressureless sintering without pressure richness A, is exactly sintering process It is not pressurized, while being rich " A " atmosphere sintering again, adding up is exactly without pressure richness A sintering.
Technical solution proposed by the present invention is: a kind of large scale MAX phase ceramics impeller preparation method, which is characterized in that packet Include following steps:
(1) MAX phase micro mist is prepared using combustion synthesis method；
(2) monomer, crosslinking agent, dispersing agent, defoaming agent are add to deionized water, are configured to premixed liquid；
(3) step (1) the MAX phase micro mist is added in step (2) described premixed liquid, ball milling mixes, and obtains injection molding slurry Material；
(4) step (3) the injection molding slurry is placed in vacuum environment, removes the bubble being mingled in slurry；
(5) it in the slurry after initiator, polymerization inhibitor, catalyst to be added to step (4) described removing bubble, stirs evenly；
(6) step (5) described slurry is cast into impeller mold under vacuum conditions, and maintains negative pressure until slurry boils It rises, entrained air bubbles is discharged, after bubble discharge, mold is taken out from vacuum environment, waits slurry polymerisation solidification；
(7) after the discharge of entrained air bubbles described in step 6, injection molding completion rear mold is taken out from vacuum environment, waits slurry Polymerizing curable；
(8) after step (7) the slurry polymerisation solidification, mold is removed, the wet base of impeller is obtained；
(9) the wet base of step (8) impeller is placed in dry liquid, until the wet base of impeller with to dry liquid humidity identical, no It is dehydrated weightlessness again；
(10) the wet base of step (9) impeller is placed in the wet temperature-controlled drying case of control, until the wet base humidity of impeller is zero, no It is dehydrated weightlessness again, obtains impeller green compact；
(11) step (10) the impeller green compact are machined, finely tune green compact size and shape；
(12) the impeller green compact after step (11) described machining are placed in vacuum degumming stove, removed contained organic in green compact Ingredient；
(13) impeller green compact after step (12) described degumming are placed in sintering furnace, complete impeller green sintering, obtains MAX phase Ceramic impeller；
(14) step (13) the MAX phase ceramics impeller is subjected to polishing refine, finely tunes impeller size shape, obtains large scale MAX phase ceramics impeller.
Further, step (1) MAX phase micro mist median (average grain diameter) D50It is 0.1~10 μm, purity is big 98.0wt%.
Further, step (2) monomer is acrylamide AM, N.N- dimethylacrylamide DMAA, metering system One of sour hydroxyl ethyl ester HEMA, methyl methacrylate MMA are that analysis is pure, and monomer accounts for the 1 of MAX phase micro powder material weight ~20wt%；Preferably acrylamide AM, analysis is pure, accounts for the 5wt% of powder weight.
The crosslinking agent is N, and N- methylene-bisacrylamide (MBAM is analyzed pure) accounts for 0.1~2wt% of powder weight, Preferably 0.5wt%.
The dispersing agent is ammonium polyacrylate (PAA-NH4) and tetramethylammonium hydroxide (TMAH) composition composite diffusion Agent, PAA-NH4Weight ratio with TMAH is 1:0~0.8, and composite dispersing agent accounts for 0.1~3wt% of powder weight, preferably 0.8wt%.
The defoaming agent is polyether antifoam agent (W-71K, analysis is pure, accounts for 0~10wt% of powder weight), preferably 2wt%.
Further, step (3) the injection molding slurry uses ammonium hydroxide to adjust slurry pH value as 9~12.
The ball milling mixing tank material is polytetrafluoroethylene (PTFE), and AC ball is mill ball, and big ball bulb diameter is about 8mm, bead ball Diameter is about 4mm, and big ball pellet quality ratio is 4:3, and the weight ratio of ratio of grinding media to material, that is, medium ball and powder is (0.5~4): 1, ball milling Revolving speed is 100~500r/min, carries out rolling ball milling；It is configured to the water based suspension that solid content is 30~60vol%, preferably 50vol%；Ball milling mixing time be 1~for 24 hours, preferably 5h.
Further, step (4) vacuum environment is the saturated vapour pressure of water at room temperature, and the boiling and exhaust time is 0.5~60min, preferably 2min.
Further, step (5) initiator is ammonium persulfate (APS, analyze pure), account for powder weight 0~ 0.5wt%.
The catalyst is N, N, N, N- tetramethylethylenediamine (TEMED, analyze pure), account for powder weight 0~ 0.5wt%.
The polymerization inhibitor is phenthazine and catechol, and the two accounts for powder weight percent and is respectively, 0.01~ 0.05wt% and 0.1~0.5wt%.
The mixing time is 0.2~5min, preferably 0.5min.
Further, step (6) vacuum environment is saturated vapour pressure at room temperature, the boiling and exhaust time is 0.5~ 60min, preferably 2min.
Further, step (7) the waiting slurry polymerisation time is 5~60min, preferably 10min.
Further, step (9) the dry liquid is the dry liquid of organic media, e.g., acetone, butanone, methanol, tetrahydro furan Mutter, ethyl alcohol, glycerine, propyl alcohol, butanol, polyethanol (PEG) etc., in dry liquid organic matter volume percent concentration be 20~ 100vol%, preferably PEG4000, concentration 40vol%.
Further, step (10) the green compact drying temperature is 20~100 DEG C, and humidity is 0~50%, preferably 80 DEG C, humidity 10%.
Further, step (12) the vacuum degumming vacuum degree is 0.1~1000Pa, preferably 10Pa；Heating rate 0.1~5 DEG C/min, preferably 0.5 DEG C/min；300~700 DEG C of degumming temperature, preferably 550 DEG C；Constant temperature time 2~20h, it is excellent It is selected as 10h.
Further, 1300~1800 DEG C of step (13) sintering temperature；0.5~10h of constant temperature time, preferably 2h；It rises Warm 2~20 DEG C/min of rate, preferably 8 DEG C/min；Sintering atmosphere is high-purity argon gas and richness A atmosphere." A " in the richness A atmosphere It is element al, in Si, P, S, Zn, Ga, Ge, As, Se, Cd, In, Sn, Sb, Ti, Pb, Bi for the neutral element of MAX phase ceramics It is one or more of；Such as, Ti3SiC ceramic sintering atmosphere is high-purity argon gas and richness Si atmosphere, Ti3AlC2Ceramic post sintering atmosphere is high-purity Argon gas and richness Al atmosphere, Ti3GeC2Ceramic post sintering atmosphere is high-purity argon gas and richness Ge atmosphere.
After method made above, the beneficial effects of the present invention are:
(1) in MAX phase Gel-casting process process, using PAA-NH4With the composite dispersing agent of TMAH composition, avoid The sedimentation of MAX phase high density slurry, and ball milling mixing process is introduced, it is conducive to powder and adsorbs composite dispersing agent.
(2) liquid phase drying process is introduced, avoids the wet base of big-size complicated shape impeller in dry initial stage cracking.
(3) in Gel-casting process, the injection molding method of vacuum pouring, boiling and exhaust is introduced, is conducive to eliminate the big ruler of casting The bubble generated when very little components is mingled with, is poured the injection moldings defect such as incomplete.
(4) the MAX phase ceramics impeller that diameter is up to 300mm can be prepared, the clothes under extremely complicated harsh environment are met Labour requires.
Detailed description of the invention
Fig. 1 is large scale MAX phase ceramics impeller preparation method process flow diagram.
Specific embodiment
In the following with reference to the drawings and specific embodiments, preparation method of the invention is further illustrated.The present invention cover it is all The MAX phase ceramics known,
Embodiment 1
As shown in Figure 1, a kind of large scale MAX phase ceramics impeller preparation method, the specific steps of which are as follows:
(1) Ti is prepared using combustion synthesis method3SiC2Micro mist；
(2) monomer, crosslinking agent, dispersing agent, defoaming agent are add to deionized water, are configured to premixed liquid；
(3) by step (1) Ti3SiC2Micro mist is added in step (2) described premixed liquid, and ball milling mixes, and obtains injection molding slurry Material；
(4) step (3) the injection molding slurry is placed in vacuum environment, removes the bubble being mingled in slurry；
(5) it in the slurry after initiator, polymerization inhibitor, catalyst to be added to step (4) described removing bubble, stirs evenly；
(6) step (5) described slurry is cast into impeller mold under vacuum conditions, and maintains negative pressure until slurry boils It rises, entrained air bubbles is discharged, after bubble discharge, mold is taken out from vacuum environment, waits slurry polymerisation solidification；
(7) after the discharge of entrained air bubbles described in step 6, injection molding completion rear mold is taken out from vacuum environment, waits slurry Polymerizing curable；
(8) after step (7) the slurry polymerisation solidification, mold is removed, the wet base of impeller is obtained；
(9) the wet base of step (8) impeller is placed in dry liquid, until the wet base of impeller is no longer dehydrated weightlessness；
(10) the wet base of step (9) impeller is placed in the wet temperature-controlled drying case of control, until the wet base of impeller is no longer dehydrated mistake Weight, obtains impeller green compact；
(11) step (10) the impeller green compact are machined, finely tune green compact size and shape；
(12) the impeller green compact after step (11) described machining are placed in vacuum degumming stove, removed contained organic in green compact Ingredient；
(13) impeller green compact after step (12) described degumming are placed in sintering furnace, complete impeller green sintering, obtains Ti3SiC2Ceramic impeller；
(14) by step (13) Ti3SiC2Ceramic impeller carries out polishing refine, finely tunes impeller size shape, obtains big ruler Very little Ti3SiC2Ceramic impeller.
Further, step (1) Ti3SiC2Micro mist median D50It is 0.5 μm, the big 98.0wt% of purity.
Step (2) monomer is acrylamide (AM), accounts for the 5wt% of powder weight.
Step (2) crosslinking agent is N, and N- methylene-bisacrylamide (MBAM is analyzed pure) accounts for powder weight 0.5wt%.
Step (2) dispersing agent is ammonium polyacrylate (PAA-NH4) and tetramethylammonium hydroxide (TMAH) composition answer Close dispersing agent, PAA-NH4Weight ratio with TMAH is 1:0.2, and composite dispersing agent accounts for the 0.8wt% of powder weight.
Step (2) defoaming agent is polyether antifoam agent, accounts for the 1.6wt% of powder weight.
Step (3) the injection molding slurry uses ammonium hydroxide to adjust slurry pH value as 9.
Step (3) the ball milling mixing tank material is polytetrafluoroethylene (PTFE), and SiC ball is mill ball, and big ball bulb diameter is about 8mm, bead bulb diameter are about 4mm, and big ball pellet quality ratio is 4:3, and the weight ratio of ratio of grinding media to material, that is, medium ball and powder is 2:1, Rotational speed of ball-mill is 500r/min, carries out rolling ball milling, is configured to the water based suspension that solid content is 50vol%；When ball milling mixes Between be 5h.
Step (4) vacuum environment is the saturated vapour pressure of water at room temperature, and the boiling and exhaust time is 1min.
Step (5) initiator is ammonium persulfate (APS is analyzed pure), accounts for the 0.01wt% of powder weight.
Step (5) polymerization inhibitor is phenthazine and catechol, and the two accounts for powder weight percent and is respectively, 0.01wt% and 0.1wt%.
Step (5) catalyst is N, N, N, and N- tetramethylethylenediamine TEMED accounts for the 0.5wt% of powder weight.
Step (5) mixing time is 0.5min.
Step (6) vacuum environment is saturated vapour pressure at room temperature, and the boiling and exhaust time is 1min.
It is 10min that the step (7), which waits the slurry polymerisation time,.
Step (9) the dry liquid is the dry liquid of organic media, e.g., acetone, butanone, methanol, tetrahydrofuran, ethyl alcohol, third Triol, propyl alcohol, butanol, polyethanol (PEG) etc., dry liquid are PEG4000, concentration 35vol%.
Step (10) the green compact drying temperature is 80 DEG C, humidity 0%.
Step (12) the vacuum degumming vacuum degree is 10Pa；0.5 DEG C/min of heating rate；600 DEG C of degumming temperature；Constant temperature Time is 6h.
Step (13) sintering temperature is 1600 DEG C；Constant temperature time 2h；10 DEG C/min of heating rate；Sintering atmosphere is height Pure argon and richness Si atmosphere.
Finally, gained Ti3SiC2Ceramic impeller, microstructure dense uniform, relative density 95%, bending strength are 420MPa, fracture toughness 6.3MPam1/2, impeller diameter 260mm meets the service demand under extreme harsh complex environment.
Embodiment 2
As shown in Figure 1, a kind of large scale MAX phase ceramics impeller preparation method, the specific steps of which are as follows:
(1) Ti is prepared using combustion synthesis method3AlC2Micro mist；
(2) monomer, crosslinking agent, dispersing agent, defoaming agent are add to deionized water, are configured to premixed liquid；
(3) by step (1) Ti3AlC2Micro mist is added in step (2) described premixed liquid, and ball milling mixes, and obtains injection molding slurry Material；
(4) step (3) the injection molding slurry is placed in vacuum environment, removes the bubble being mingled in slurry；
(5) it in the slurry after initiator, polymerization inhibitor to be added to step (4) described removing bubble, stirs evenly；
(6) step (5) described slurry is cast into impeller mold under vacuum conditions, and maintains negative pressure until slurry boils It rises, entrained air bubbles is discharged, after bubble discharge, mold is taken out from vacuum environment, waits slurry polymerisation solidification；
(7) after the discharge of entrained air bubbles described in step 6, injection molding completion rear mold is taken out from vacuum environment, waits slurry Polymerizing curable；
(8) after step (7) the slurry polymerisation solidification, mold is removed, the wet base of impeller is obtained；
(9) the wet base of step (8) impeller is placed in dry liquid, until the wet base of impeller is no longer dehydrated weightlessness；
(10) the wet base of step (9) impeller is placed in the wet temperature-controlled drying case of control, until the wet base of impeller is no longer dehydrated mistake Weight, obtains impeller green compact；
(11) step (10) the impeller green compact are machined, finely tune green compact size and shape；
(12) the impeller green compact after step (11) described machining are placed in vacuum degumming stove, removed contained organic in green compact Ingredient；
(13) impeller green compact after step (12) described degumming are placed in sintering furnace, complete impeller green sintering, obtains Ti3AlC2Ceramic impeller；
(14) by step (13) Ti3AlC2Ceramic impeller carries out polishing refine, finely tunes impeller size shape, obtains liquid Lead bismuth alloy coolant pump Ti3AlC2Ceramic impeller.
Further, step (1) Ti3AlC2Micro mist median D50It is 0.5 μm, the big 98.0wt% of purity.
Step (2) monomer is acrylamide (AM), accounts for the 5wt% of powder weight.
Step (2) crosslinking agent is N, and N- methylene-bisacrylamide (MBAM is analyzed pure) accounts for powder weight 0.5wt%.
Step (2) dispersing agent is ammonium polyacrylate (PAA-NH4) and tetramethylammonium hydroxide (TMAH) composition answer Close dispersing agent, PAA-NH4Weight ratio with TMAH is 1:0.3, and composite dispersing agent accounts for the 0.9wt% of powder weight.
Step (2) defoaming agent is polyether antifoam agent, accounts for the 1.2wt% of powder weight.
Step (3) the injection molding slurry uses ammonium hydroxide to adjust slurry pH value as 9.
Step (3) the ball milling mixing tank material is polytetrafluoroethylene (PTFE), and SiC ball is mill ball, and big ball bulb diameter is about 8mm, bead bulb diameter are about 4mm, and big ball pellet quality ratio is 4:3, and the weight ratio of ratio of grinding media to material, that is, medium ball and powder is 2:1, Rotational speed of ball-mill is 500r/min, carries out rolling ball milling, is configured to the water based suspension that solid content is 50vol%；When ball milling mixes Between be 5h.
Step (4) vacuum environment is the saturated vapour pressure of water at room temperature, and the boiling and exhaust time is 1min.
Step (5) initiator is ammonium persulfate (APS is analyzed pure), accounts for the 0.01wt% of powder weight.
Step (5) polymerization inhibitor is phenthazine and catechol, and the two accounts for powder weight percent and is respectively, 0.01wt% and 0.1wt%, is added without catalyst.
Step (5) mixing time is 0.5min.
Step (6) vacuum environment is saturated vapour pressure at room temperature, and the boiling and exhaust time is 1min.
It is 10min that the step (7), which waits the slurry polymerisation time,.
Step (9) the dry liquid is the dry liquid of organic media, e.g., acetone, butanone, methanol, tetrahydrofuran, ethyl alcohol, third Triol, propyl alcohol, butanol, polyethanol (PEG) etc., dry liquid are PEG4000, concentration 40vol%.
Step (10) the green compact drying temperature is 80 DEG C, humidity 0%.
Step (12) the vacuum degumming vacuum degree is 10Pa；0.5 DEG C/min of heating rate；600 DEG C of degumming temperature；Constant temperature Time is 6h.
Step (13) sintering temperature is 1550 DEG C；Constant temperature time 2h；10 DEG C/min of heating rate；Sintering atmosphere is height Pure argon and richness Al atmosphere.
Finally, gained Ti3AlC2Ceramic impeller, microstructure dense uniform, relative density 95.5%, bending strength are 370MPa, fracture toughness 5.8MPam1/2, impeller diameter 285mm meets the service demand under extreme harsh complex environment.
Embodiment 3
As shown in Figure 1, a kind of large scale MAX phase ceramics impeller preparation method, the specific steps of which are as follows:
(1) Ti is prepared using combustion synthesis method2AlC micro mist；
(2) monomer, crosslinking agent, dispersing agent, defoaming agent are add to deionized water, are configured to premixed liquid；
(3) by step (1) Ti2AlC micro mist is added in step (2) described premixed liquid, and ball milling mixes, and obtains injection molding slurry Material；
(4) step (3) the injection molding slurry is placed in vacuum environment, removes the bubble being mingled in slurry；
(5) it in the slurry after initiator, polymerization inhibitor to be added to step (4) described removing bubble, stirs evenly；
(6) step (5) described slurry is cast into impeller mold under vacuum conditions, and maintains negative pressure until slurry boils It rises, entrained air bubbles is discharged, after bubble discharge, mold is taken out from vacuum environment, waits slurry polymerisation solidification；
(7) after the discharge of entrained air bubbles described in step 6, injection molding completion rear mold is taken out from vacuum environment, waits slurry Polymerizing curable；
(8) after step (7) the slurry polymerisation solidification, mold is removed, the wet base of impeller is obtained；
(9) the wet base of step (8) impeller is placed in dry liquid, until the wet base of impeller is no longer dehydrated weightlessness；
(10) the wet base of step (9) impeller is placed in the wet temperature-controlled drying case of control, until the wet base of impeller is no longer dehydrated mistake Weight, obtains impeller green compact；
(11) step (10) the impeller green compact are machined, finely tune green compact size and shape；
(12) the impeller green compact after step (11) described machining are placed in vacuum degumming stove, removed contained organic in green compact Ingredient；
(13) impeller green compact after step (12) described degumming are placed in sintering furnace, complete impeller green sintering, obtains Ti2AlC ceramic impeller；
(14) by step (13) Ti2AlC ceramic impeller carries out polishing refine, finely tunes impeller size shape, obtains big ruler Very little Ti2AlC ceramic impeller.
Further, step (1) Ti2AlC micro mist median D50It is 0.5 μm, the big 98.0wt% of purity.
Step (2) monomer is acrylamide (AM), accounts for the 5wt% of powder weight.
Step (2) crosslinking agent is N, and N- methylene-bisacrylamide (MBAM is analyzed pure) accounts for powder weight 0.5wt%.
Step (2) dispersing agent is ammonium polyacrylate (PAA-NH4) and tetramethylammonium hydroxide (TMAH) composition answer Close dispersing agent, PAA-NH4Weight ratio with TMAH is 1:0.3, and composite dispersing agent accounts for the 0.9wt% of powder weight.
Step (2) defoaming agent is polyether antifoam agent, accounts for the 1.2wt% of powder weight.
Step (3) the injection molding slurry uses ammonium hydroxide to adjust slurry pH value as 9.
Step (3) the ball milling mixing tank material is polytetrafluoroethylene (PTFE), and SiC ball is mill ball, and big ball bulb diameter is about 8mm, bead bulb diameter are about 4mm, and big ball pellet quality ratio is 4:3, and the weight ratio of ratio of grinding media to material, that is, medium ball and powder is 2:1, Rotational speed of ball-mill is 500r/min, carries out rolling ball milling, is configured to the water based suspension that solid content is 50vol%；When ball milling mixes Between be 5h.
Step (4) vacuum environment is the saturated vapour pressure of water at room temperature, and the boiling and exhaust time is 1min.
Step (5) initiator is ammonium persulfate (APS is analyzed pure), accounts for the 0.01wt% of powder weight.
Step (5) polymerization inhibitor is phenthazine and catechol, and the two accounts for powder weight percent and is respectively, 0.01wt% and 0.1wt%, is added without catalyst.
Step (5) mixing time is 0.5min.
Step (6) vacuum environment is saturated vapour pressure at room temperature, and the boiling and exhaust time is 1min.
It is 10min that the step (7), which waits the slurry polymerisation time,.
Step (9) the dry liquid is the dry liquid of organic media, e.g., acetone, butanone, methanol, tetrahydrofuran, ethyl alcohol, third Triol, propyl alcohol, butanol, polyethanol (PEG) etc., dry liquid are PEG4000, concentration 40vol%.
Step (10) the green compact drying temperature is 80 DEG C, humidity 0%.
Step (12) the vacuum degumming vacuum degree is 10Pa；0.5 DEG C/min of heating rate；600 DEG C of degumming temperature；Constant temperature Time is 6h.
Step (13) sintering temperature is 1550 DEG C；Constant temperature time 2h；10 DEG C/min of heating rate；Sintering atmosphere is height Pure argon and richness Al atmosphere.
Finally, gained Ti2AlC ceramic impeller, microstructure dense uniform, relative density 95.7%, bending strength are 460MPa, fracture toughness 7.2MPam1/2, impeller diameter 280mm meets the service demand under extreme harsh complex environment.
Embodiment 4
As shown in Figure 1, a kind of large scale MAX ceramic impeller preparation method, the specific steps of which are as follows:
(1) Nb is prepared using combustion synthesis method4AlC3Micro mist；
(2) monomer, crosslinking agent, dispersing agent, defoaming agent are add to deionized water, are configured to premixed liquid；
(3) by step (1) Nb4AlC3Micro mist is added in step (2) described premixed liquid, and ball milling mixes, and obtains injection molding slurry Material；
(4) step (3) the injection molding slurry is placed in vacuum environment, removes the bubble being mingled in slurry；
(5) it in the slurry after initiator, polymerization inhibitor to be added to step (4) described removing bubble, stirs evenly；
(6) step (5) described slurry is cast into impeller mold under vacuum conditions, and maintains negative pressure until slurry boils It rises, entrained air bubbles is discharged, after bubble discharge, mold is taken out from vacuum environment, waits slurry polymerisation solidification；
(7) after the discharge of entrained air bubbles described in step 6, injection molding completion rear mold is taken out from vacuum environment, waits slurry Polymerizing curable；
(8) after step (7) the slurry polymerisation solidification, mold is removed, the wet base of impeller is obtained；
(9) the wet base of step (8) impeller is placed in dry liquid, until the wet base of impeller is no longer dehydrated weightlessness；
(10) the wet base of step (9) impeller is placed in the wet temperature-controlled drying case of control, until the wet base of impeller is no longer dehydrated mistake Weight, obtains impeller green compact；
(11) step (10) the impeller green compact are machined, finely tune green compact size and shape；
(12) the impeller green compact after step (11) described machining are placed in vacuum degumming stove, removed contained organic in green compact Ingredient；
(13) impeller green compact after step (12) described degumming are placed in sintering furnace, complete impeller green sintering, obtains Nb4AlC3Ceramic impeller；
(14) by step (13) Nb4AlC3Ceramic impeller carries out polishing refine, finely tunes impeller size shape, obtains big ruler Very little Nb4AlC3Ceramic impeller.
Further, step (1) Nb4AlC3Micro mist median D50It is 0.5 μm, the big 98.0wt% of purity.
Step (2) monomer is acrylamide (AM), accounts for the 5wt% of powder weight.
Step (2) crosslinking agent is N, and N- methylene-bisacrylamide (MBAM is analyzed pure) accounts for powder weight 0.5wt%.
Step (2) dispersing agent is ammonium polyacrylate (PAA-NH4) and tetramethylammonium hydroxide (TMAH) composition answer Close dispersing agent, PAA-NH4Weight ratio with TMAH is 1:0.3, and composite dispersing agent accounts for the 0.9wt% of powder weight.
Step (2) defoaming agent is polyether antifoam agent, accounts for the 1.2wt% of powder weight.
Step (3) the injection molding slurry uses ammonium hydroxide to adjust slurry pH value as 9.
Step (3) the ball milling mixing tank material is polytetrafluoroethylene (PTFE), and SiC ball is mill ball, and big ball bulb diameter is about 8mm, bead bulb diameter are about 4mm, and big ball pellet quality ratio is 4:3, and the weight ratio of ratio of grinding media to material, that is, medium ball and powder is 2:1, Rotational speed of ball-mill is 500r/min, carries out rolling ball milling, is configured to the water based suspension that solid content is 50vol%；When ball milling mixes Between be 5h.
Step (4) vacuum environment is the saturated vapour pressure of water at room temperature, and the boiling and exhaust time is 1min.
Step (5) initiator is ammonium persulfate (APS is analyzed pure), accounts for the 0.01wt% of powder weight.
Step (5) polymerization inhibitor is phenthazine and catechol, and the two accounts for powder weight percent and is respectively, 0.01wt% and 0.1wt%, is added without catalyst.
Step (5) mixing time is 0.5min.
Step (6) vacuum environment is saturated vapour pressure at room temperature, and the boiling and exhaust time is 1min.
It is 10min that the step (7), which waits the slurry polymerisation time,.
Step (9) the dry liquid is the dry liquid of organic media, e.g., acetone, butanone, methanol, tetrahydrofuran, ethyl alcohol, third Triol, propyl alcohol, butanol, polyethanol (PEG) etc., dry liquid are PEG4000, concentration 40vol%.
Step (10) the green compact drying temperature is 80 DEG C, humidity 0%.
Step (12) the vacuum degumming vacuum degree is 10Pa；0.5 DEG C/min of heating rate；600 DEG C of degumming temperature；Constant temperature Time is 6h.
Step (13) sintering temperature is 1700 DEG C；Constant temperature time 2h；10 DEG C/min of heating rate；Sintering atmosphere is height Pure argon and richness Al atmosphere.
Finally, gained Nb4AlC3Ceramic impeller, microstructure dense uniform, relative density 95.7%, bending strength are 320MPa, fracture toughness 6.3MPam1/2, impeller diameter 290mm, good corrosion resistance meets under extreme harsh complex environment Service demand.
A kind of large scale MAX phase ceramics impeller preparation method of the present invention covers all known MAX phase ceramics, The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technical staff of the industry should Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention Reason, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes and improvements It all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent circle It is fixed.

Claims (12)

1. a kind of large scale MAX phase ceramics impeller preparation method, which comprises the steps of:
(1) MAX phase micro mist is prepared using combustion synthesis method；
(2) monomer, crosslinking agent, dispersing agent, defoaming agent are add to deionized water, are configured to premixed liquid；
(3) step (1) the MAX phase micro mist is added in step (2) described premixed liquid, ball milling mixes, and obtains injection molding slurry；
(4) step (3) the injection molding slurry is placed in vacuum environment, removes the bubble being mingled in slurry；
(5) it in the slurry after initiator, polymerization inhibitor, catalyst to be added to step (4) described removing bubble, stirs evenly；
(6) step (5) described slurry is cast into impeller mold under vacuum conditions, and negative pressure is maintained to boil up to slurry, Entrained air bubbles are discharged, after bubble discharge, mold is taken out from vacuum environment, waits slurry polymerisation solidification；
(7) after the discharge of entrained air bubbles described in step 6, injection molding completion rear mold is taken out from vacuum environment, waits slurry polymerisation Solidification；
(8) after step (7) the slurry polymerisation solidification, mold is removed, the wet base of impeller is obtained；
(9) the wet base of step (8) impeller is placed in dry liquid, until the wet base of impeller is identical as dry liquid humidity, no longer de- Water is weightless；
(10) the wet base of step (9) impeller is placed in the wet temperature-controlled drying case of control, until the wet base humidity of impeller is zero, no longer takes off Water is weightless, obtains impeller green compact；
(11) step (10) the impeller green compact are machined, finely tune green compact size and shape；
(12) the impeller green compact after step (11) described machining are placed in vacuum degumming stove, remove in green compact it is contained it is organic at Point；
(13) impeller green compact after step (12) described degumming are placed in sintering furnace, complete impeller green sintering, obtains MAX phase ceramics Impeller；
(14) step (13) the MAX phase ceramics impeller is subjected to polishing refine, finely tunes impeller size shape, obtains large scale MAX Phase ceramics impeller.
2. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that:
Step (1) the MAX phase micro mist average grain diameter D50It is 0.1~10 μm, the big 98.0wt% of purity.
3. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: step (2) described list Body is acrylamide AM, N.N- dimethylacrylamide DMAA, hydroxyethyl methacrylate HEMA, methyl methacrylate MMA One of, it is that analysis is pure, and monomer accounts for 1~20wt% of MAX phase micro powder material weight；
The crosslinking agent be N, N- methylene-bisacrylamide MBAM, analyze it is pure, account for MAX phase micro powder material weight 0.1~ 2wt%；
The dispersing agent is ammonium polyacrylate PAA-NH4With the composite dispersing agent of tetramethylammonium hydroxide TMAH composition, PAA-NH4 Weight ratio with TMAH is 1:0~0.8, and composite dispersing agent accounts for 0.1~3wt% of MAX phase micro powder material weight；
The defoaming agent is polyether antifoam agent W-71K, and analysis is pure, accounts for 0~10wt% of MAX phase micro powder material weight.
4. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: step (3) described note Mould slurry uses ammonium hydroxide to adjust slurry pH value as 9~12；
Step (3) the ball milling mixing tank material is polytetrafluoroethylene (PTFE), and AC ball is mill ball, and big ball bulb diameter is 8mm, bead ball Diameter is 4mm, and big ball pellet quality ratio is 4:3, and the weight ratio of ratio of grinding media to material, that is, medium ball and powder is (0.5~4): 1, ball milling turns Speed is 100~500r/min, carries out rolling ball milling；It is configured to the water based suspension that solid content is 30~60vol%.
5. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: step (4) is described true Altitude is the saturated vapour pressure of water at room temperature, and the boiling and exhaust time is 0.5~60min.
6. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: step (5) is described to draw Hair agent is ammonium persulfate APS, and analysis is pure, accounts for 0~0.5wt% of MAX phase micro powder material weight；
The catalyst be N, N, N, N- tetramethylethylenediamine TEMED, analyze it is pure, account for MAX phase micro powder material weight 0~ 0.5wt%；
The polymerization inhibitor is phenthazine and catechol, and the two accounts for MAX phase micro powder material weight percent and is respectively, 0.01~ 0.05wt% and 0.1~0.5wt%；
The mixing time is 0.2~5min.
7. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: step (6) is described true Altitude is saturated vapour pressure at room temperature, and the boiling and exhaust time is 0.5~60min.
8. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: step (7) is described etc. It is 5~60min to the slurry polymerisation time.
9. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: step (9) is described dry Liquid drier is that the dry liquid of organic media includes acetone, butanone, methanol, tetrahydrofuran, ethyl alcohol, glycerine, propyl alcohol, butanol, polyethanol PEG, drying organic matter volume percent concentration in liquid is 20~100vol%.
10. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: the step (10) Green compact drying temperature is 20~100 DEG C, and humidity is 0~50%.
11. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: step (12) is described Vacuum degumming vacuum degree is 0.1~1000Pa, 0.1~5 DEG C/min of heating rate；300~700 DEG C of degumming temperature；Constant temperature time 2 ~20h.
12. large scale MAX phase ceramics impeller preparation method according to claim 1, it is characterised in that: step (13) is described 1300~1800 DEG C of sintering temperature, 0.5~10h of constant temperature time；2~20 DEG C/min of heating rate, sintering atmosphere are high-purity argon gas With rich A atmosphere, " A " in the richness A atmosphere is the neutral element of MAX phase ceramics, be element al, Si, P, S, Zn, Ga, Ge, One or more of As, Se, Cd, In, Sn, Sb, Ti, Pb, Bi；Ti3SiC ceramic sintering atmosphere is high-purity argon gas and richness Si gas Atmosphere, Ti3AlC2Ceramic post sintering atmosphere is high-purity argon gas and richness Al atmosphere, Ti3GeC2Ceramic post sintering atmosphere is high-purity argon gas and richness Ge Atmosphere.
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