CN108218462A - Resin based sizing and SiC ceramic reaction forming method - Google Patents
Resin based sizing and SiC ceramic reaction forming method Download PDFInfo
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- CN108218462A CN108218462A CN201611199949.4A CN201611199949A CN108218462A CN 108218462 A CN108218462 A CN 108218462A CN 201611199949 A CN201611199949 A CN 201611199949A CN 108218462 A CN108218462 A CN 108218462A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/003—Joining burned ceramic articles with other burned ceramic articles or other articles by heating by means of an interlayer consisting of a combination of materials selected from glass, or ceramic material with metals, metal oxides or metal salts
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/02—Aspects relating to interlayers, e.g. used to join ceramic articles with other articles by heating
- C04B2237/04—Ceramic interlayers
- C04B2237/08—Non-oxidic interlayers
- C04B2237/083—Carbide interlayers, e.g. silicon carbide interlayers
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
- C04B2237/36—Non-oxidic
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/32—Ceramic
- C04B2237/36—Non-oxidic
- C04B2237/365—Silicon carbide
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- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/55—Pre-treatments of a coated or not coated substrate other than oxidation treatment in order to form an active joining layer
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Abstract
The present invention relates to resin based sizing and SiC ceramic reaction forming method, the resin based sizing includes：Weight percentage, resin 25~35%, organic solvent 25~35% and silicon carbide micro-powder 30~50%.The present invention uses resin as carbon source, as binding agent, the porous structure of uniform pore diameter distribution generated after being cracked due to resin so that connection layer defects are reduced, and are conducive to the raising of switching performance.
Description
Technical field
The present invention relates to ceramic material field, more particularly to a kind of resin based sizing and silicon carbide ceramics reaction forming side
Method.
Background technology
Silicon carbide ceramics has good elevated temperature strength, and low thermal coefficient of expansion, excellent thermal shock resistance is corrosion-resistant, resistance to
Abrasion, is widely used in fields such as aerospace, oil, chemical industry, machineries, is increasingly taken seriously at present.But it is carbonized
High brittleness, the low ductility of silicon ceramics, high rigidity make its processing performance poor, to manufacture complex devices difficulty it is larger, cost compared with
It is high.Thus, it is a kind of effective method to be connected simple components by interconnection technique.
The main method for being presently used for silicon carbide ceramics connection has：Active metal brazing is connected with diffusion welding (DW), Transient liquid phase
Connect (TLPB), SHS process (SHS) connection, precursor connection, reaction forming etc..Solder bonding metal connection it is main not
Foot is that connector coefficient of thermal expansion mismatches generation thermal stress with base material, reduces bonding strength, and high temperature conjunction poor-performing.From climing
The reaction speed for prolonging high―temperature nuclei (SHS) connection is too fast, and solder burning time is difficult to control, so as to also just be difficult to interfacial reaction
Control.More precursor connection was studied in recent years, and connection layer porosity is larger after Pintsch process, not fine and close, causes connection strong
Degree is not high.Reaction forming grows up from SiC reaction moldings, is currently used primarily in connection SiC ceramic and fiber reinforcement
Composite material.The major advantage of reaction forming method is by the design to linkage interface ingredient and structure so that articulamentum
The performances such as mechanics, calorifics can be in close proximity to connected base material basis material.A kind of successful reaction forming technology of comparison is
The technology that the Lewis research centers of NASA are succeeded in developing：To first contain carbon compound be placed in connector area (usual carbon compound with
The form of slurry form or casting films adds in), by test specimen in fixture, dry 10~20min between 110~120 DEG C,
Welded part is made to bond together.Si or alloy containing Si are done into slabbing, paste or suspension again and are put into joint area, Ran Hougen
1250~1425 DEG C of 5~10min of heat preservation are heated to according to infiltration type, Si the or Si alloys of fusing penetrate under capillary force action
It is reacted into middle layer biscuit and with carbon, generates new SiC and realization and the connection of matrix, middle layer also have trip in addition to SiC
Exist from silicon.Carbon compound used in the prior art is mainly the solid carbon sources such as carbon black, graphite powder, carbon cloth.
Porous structure is uneven after reaction forming technique connection is cracked due to carbon compound carbonization, leads to siliconising process
It is middle to lead to occur inhomogeneities and the undesirable contraction occurred in final material so that articulamentum occurs with parent material interface
The defects of crack, gap, causes post-production difficult, and finished product has the defects of apparent connection gap.Patent
SiC is generated by silicon carbide precursor in 201310040858.6, apparent body is had after such reaction in-situ method generation SiC
Product is shunk, and generates larger hole.
Invention content
In view of the above-mentioned defects in the prior art, the purpose of the present invention is to provide a kind of junctions and the structural behaviour of base material
Unanimously, it the precision of material and has good uniformity, connects layer thickness and the controllable silicon carbide ceramics reaction forming of uniform texture
Method, realization are stably connected with.
Here, the present invention provides a kind of resin based sizing, the resin based sizing includes：
Weight percentage, resin 25~35%, organic solvent 25~35% and silicon carbide micro-powder 30~50%.It is described
Resin based sizing can be used as the binder of silicon carbide ceramics reaction forming.
Preferably, the resin based sizing further includes the carbon black of 0~10wt%.
Preferably, the resin based sizing further includes the dispersant of 4~5wt%, and/or the curing agent of 2~10wt%.
Preferably, the resin is organic carbonaceous resin, preferably phenolic resin and/or furfuryl alcohol resin.The organic solvent
For alcohols, preferably at least one of ethyl alcohol, ethylene glycol, polyethylene glycol, diglycol, three contracting triethylene glycols.
Preferably, the dispersant is selected from least one of polyvinylpyrrolidone, polyacrylamide, phosphate.Institute
Benzene sulfonyl chloride and/or hexa can be selected from by stating curing agent.
The present invention also provides a kind of preparation method of above-mentioned resin based sizing, including：Organic solvent is mixed with resin
To resin solution；Silicon carbide micro-powder (or silicon carbide micro-powder+carbon black) with resin solution is mixed, and adds dispersant, curing
Agent obtains the resin based sizing.
The present invention also provides a kind of silicon carbide ceramics reaction forming method, the method is using above-mentioned resin based sizing as connection
Material connection silicon carbide ceramic components, including：
At least two silicon carbide ceramic components are connected into complex by least one joint face, are connected in silicon carbide ceramic components
Above-mentioned resin based sizing is coated between junction, cure under pressure, cracking unsticking is carried out, obtains pre-connection part；
The position that is at least connected with of the pre-connection part is buried into silicon source, melts at a temperature of 1400~1700 DEG C and oozes processing, it is raw
It is connected into articulamentum with realizing.
The present invention by the carbon in pyroreaction binder and silicon or siliceous is mixed using resin based sizing as binder
Object reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.Compared with prior art, the present invention
The present invention, as main body carbon source, has certain caking property, high temperature siliconising is not required to clamping mould, simplifies production work using resin
Skill.Resin used in the present invention can generate the uniform porous structure of pore structure after cracking.Also, the connection method of the present invention obtains
It is SiC phases to connection layer main body, consistent with the structural behaviour of SiC ceramic matrix, hot physical property matching is preferable, can obtain high temperature resistant
The jointing haveing excellent performance.In addition, connection layer thickness and uniform texture are controllable, switching performance stability is high.According to this
The articulamentum of invention is connect with parent material interface densification.The present invention uses resin as carbon source, as binding agent, since resin cracks
The porous structure of uniform pore diameter distribution generated afterwards so that connection layer defects are reduced, and are conducive to the raising of switching performance.Connection temperature
The raising of degree contributes to the infiltration of molten silicon, conducive to the progress of silicon-carbon reaction.In addition, it is filled out by adding inertia in slurry is connected
Material silicon carbide micro-powder can effectively control the contraction in connection procedure, it is possible to reduce defect generates.The silicon carbide ceramics of the present invention
Reaction forming method reduces difficulty of processing, simplifies process, cost-effective, and connects the structural behaviour of layer material and base material
Unanimously, the occasion available for carrying high temperature application.
Preferably, the pressure of the pressurization is in 0.1~0.5MPa.
Preferably, the cured temperature schedule is gradient increased temperature, start to keep the temperature after being preferably warming up to 70~90 DEG C, so
It often increases 20 DEG C afterwards and keeps the temperature 2~6 hours, until 110~130 DEG C.
Preferably, the cracking unsticking temperature is 900-1200 DEG C, heating rate is 1~2.5 DEG C/min.
The silicon source at least contains elemental silicon, is preferably made of pure silicon or silicon and refractory metal, refractory metal for example tungsten, tantalum,
Molybdenum, niobium, hafnium etc., refractory metal additive amount in the silicon source is 0~10%.
Preferably, it is described melt ooze processing temperature be 1450~1650 DEG C.
Preferably, it is described melt ooze processing time be 10~30 minutes.
In the present invention, the articulamentum is ceramic of compact articulamentum of the thickness at 5-200 μm, and the thickness of preferably articulamentum is
10~50 microns.
Description of the drawings
Fig. 1 is that the embodiment of the present invention 2 connects sample joint microstructure morphology scanning electron microscope image, and the right and left is
SiC ceramic matrix, centre are articulamentum, and wherein white area is the SiC phases of addition, and light gray areas is newly-generated for reaction in-situ
SiC phases, dark gray areas is free silica；
Fig. 2 is that the embodiment of the present invention 3 connects sample joint microstructure morphology scanning electron microscope image, and the right and left is made pottery for SiC
Porcelain basal body, centre are articulamentum, and wherein white area is the SiC phases of addition, and light gray areas is the newly-generated SiC of reaction in-situ
Phase, dark gray areas are free silica.
Specific embodiment
It is further illustrated the present invention below in conjunction with attached drawing and following embodiments, it should be appreciated that following embodiments are only used for
Illustrate the present invention, be not intended to limit the present invention.
The present invention provides a kind of methods for the silicon carbide ceramics reaction forming for connecting layer thickness and forming uniform, controllable.This
Invention prepares binder using organic resin as carbon source, coated with resins base binder (the i.e. resin base between two ceramic components
Slurry), carry out pressure curing, cracking carbonization, then melt siliconising or siliceous mixture at high temperature so that carbon in binder with
Silicon or siliceous mixture reaction generation ceramic of compact articulamentum, so as to fulfill being stably connected with.The silicon carbide ceramics reaction of the present invention
Connection method reduces difficulty of processing, simplifies process, cost-effective, and connects the structural behaviour one of layer material and base material
It causes, the occasion available for carrying high temperature application.
Hereinafter, illustrate the silicon carbide ceramics reaction forming method of the present invention.
First, prepare ceramic component to be connected, carry out pre-treatment.As an example, pre-treatment can for example include：
Prepare at least two silicon carbide ceramics samples (i.e. silicon carbide ceramic components), and will treat that joint face grinding is smooth, by the carbon of milled
SiClx ceramic sample is positioned over 10~20min of ultrasonic cleaning in alcohol, places oven drying, stays standby for use.
Then, it is assembled and pre-connection.It can specifically include at least two silicon carbide ceramics samples passing through at least one
A joint face connects into a complex, and the resin base binder prepared is coated between silicon carbide ceramics joint face, carries out
Cure under pressure, cracking unsticking, obtain pre-connection part.As an example, such as by two silicon carbide ceramics samples pass through one
Joint face connects into a complex, in the company of the joint face and another silicon carbide ceramics sample of a silicon carbide ceramics sample
Coated with resins base binder between junction carries out cure under pressure, cracking unsticking, obtains pre-connection part.
In the present invention, resin base binder can include following principal component：Resin, organic solvent and silicon carbide micro-powder.
In addition, resin base binder can also include suitable dispersant and curing agent.
Wherein, resin includes but not limited to the organic carbonaceous resin such as phenolic resin, furfuryl alcohol resin.The weight of resin in principal component
Measuring percentage composition can be in 25-35%.The weight percentage of resin has and disclosure satisfy that caking property simultaneously in 25-35%
The advantages of enough carbon sources are provided.The present invention is using resin as carbon source, as binding agent, the hole generated after being cracked due to resin
The equally distributed porous structure of diameter so that connection layer defects are reduced, and are conducive to the raising of switching performance.The raising of connection temperature has
Help the infiltration of molten silicon, conducive to the progress of silicon-carbon reaction.
Organic solvent includes but not limited to ethyl alcohol, ethylene glycol, polyethylene glycol, diglycol, three contracting triethylene glycols etc..
The weight percentage of organic solvent can be in 25-35% in principal component.
In principal component the weight percentage of silicon carbide micro-powder can in 30-50%, preferably greater than 30% and be 50%
Below.The increase of SiC powder contents contributes to the raising of switching performance and connective stability, and excessively high SiC micro mists can cause
Slurry viscosity is excessive or can not be into slurry.It can the effective company of control by adding inert filler silicon carbide micro-powder in slurry is connected
Contraction in termination process, it is possible to reduce defect generates.In addition, the carbon of 0-10% (preferably 2~5%) can also be included in principal component
It is black, add in irregular hole filling after carbon black can crack resin so that pore structure is evenly.
Dispersant includes but not limited to polyvinylpyrrolidone, polyacrylamide, phosphate etc..The usage amount of dispersant can
Think the 4-5% of principal component total amount (total weight).Curing agent includes but not limited to benzene sulfonyl chloride, hexa etc..Curing
The usage amount of agent can be 2~10% (such as 4%) of principal component total amount.
The preparation method of resin base binder can include：Organic solvent is mixed with resin, stirring is allowed to fully dissolve,
It is configured to resin solution；Silicon carbide micro-powder (or silicon carbide micro-powder and carbon black) with resin solution is mixed, is configured to slurry；Addition
Dispersant, curing agent, then carry out ball milling to slurry, and vacuum degassing obtains binder.Wherein, Ball-milling Time can be 6~
12h, rotating speed can be 250~350r/min (such as 300r/min).
In this implementation form, which is used for silicon carbide ceramics reaction forming, but not limited to this, the tree
Aliphatic radical binder can be used for the connection of other ceramic materials, such as silicon nitride ceramics, aluminium nitride ceramics.
In the present invention, the pressure of pressurized treatments can be in 0.1-0.5MPa.Gradient increased temperature may be used in solidification temperature system,
It is preferred that starting to keep the temperature after being warming up to 70~90 DEG C, then often increasing 20 DEG C keeps the temperature 2~6 hours, until 110~130 DEG C.As
One example, the solidification temperature system are, for example,：80 DEG C of heat preservations 4h, 100 DEG C of heat preservations 4h, 120 DEG C of heat preservation 4h.
In the present invention, cracking unsticking temperature can be at 900-1200 DEG C (such as 900 DEG C), and heating rate can be 1~2.5
DEG C/min (such as 2 DEG C/min).In addition, cracking unsticking can carry out under an ar atmosphere.During unsticking is cracked, pitch shake
It solves as carbon.
Then, above-mentioned pre-connection part is melted into siliconising or siliceous mixture at high temperature.Specifically, can include will be above-mentioned pre-
Connector (being at least connected with position) is buried into silicon (pure silicon) or siliceous mixture, at a temperature of 1400~1700 DEG C keep the temperature 10~
30min, which melts, oozes processing so that the carbon in binder reacts generation articulamentum with silicon or siliceous mixture, connects so as to fulfill stablizing
It connects.Compared with generating SiC by silicon carbide precursor in the prior art, after the method for the present invention generates silicon carbide by external siliconising
Volume expansion, and porous carbon structure hole is filled, extra hole is filled by free silica, therefore will not generate a large amount of holes.
In the present invention, siliceous mixture can be made of silicon and refractory metal.Wherein the content of silicon can be 0~100wt%,
The content of refractory metal can be 0~10wt%.The refractory metal can be the metal that fusing point is 1700 DEG C or more, for example, tungsten, tantalum,
Molybdenum, niobium, hafnium etc..Pre-connection part, which is buried, can generate the metal carbides in addition to silicon carbide into siliceous mixture, improve connection
Layer consistency, improves articulamentum performance.Each component content can be according to carbon in the connecting portion of pre-connection part in siliceous mixture
Content determines, that is, can be the amount that generation SiC at least can be reacted with whole carbon.
In a preferred embodiment, pre-connection part is buried into siliceous mixture, is protected at a temperature of 1450~1650 DEG C
10~30min of temperature, which melts, oozes processing.
According to the above method, the silicon carbide ceramics connected.Reaction between the silicon carbide ceramics connected in this way
Articulamentum is using silicon carbide as main phase, the newly-generated SiC phases (β-SiC phases) of the SiC phases (α-SiC phases) including addition, reaction in-situ,
Free silica is additionally included, contents of free si corrodes sample by HF acid front and rear weight difference and calculates, contents of free si 10
~35%.The reaction forming layer is thickness in 5-200 μm of controllable ceramic of compact articulamentum.
Advantages of the present invention：
Using resin as main body carbon source, there is certain caking property, i.e. resin doubles as carbon source and binding agent, and high temperature siliconising is not required to
Clamping mould simplifies production technology；
It is SiC phases that connection layer main body, which is prepared, consistent with the structural behaviour of SiC ceramic matrix, and the matching of hot physical property is preferable, can be with
Obtain the excellent jointing of high temperature resistance；
It connects layer thickness and uniform texture is controllable, switching performance stability is high；
The silicon carbide ceramics reaction forming method of the present invention reduces difficulty of processing, simplifies process, cost-effective, and articulamentum
Material is consistent with the structural behaviour of base material, the occasion available for carrying high temperature application.
Embodiment is enumerated further below so that the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.
Embodiment 1
1) pre-treatment：Prepare at least two silicon carbide ceramics samples, and will treat that joint face grinding is smooth, the silicon carbide of milled is made pottery
Porcelain sample is positioned over 10~20min of ultrasonic cleaning in alcohol, places oven drying, stays standby for use；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：Phenolic resin 30%, ethyl alcohol 30%, silicon carbide micro-powder 40%；And point of the weight for principal component total amount 4%
Powder polyethylene pyrrole network alkanone, weight are the curing agent benzene sulfonyl chloride of principal component total amount 4%；
A. 15g resins are added in 15g organic solvents, stirring is allowed to fully dissolve, and resin solution is configured；
B. 20g silicon carbide micro-powders are added in resin solution, are configured to slurry；
C. addition 2g dispersants, 2g curing agent, then carry out slurry ball milling, Ball-milling Time 6h, rotating speed 300r/min, very
Empty degasification obtains resin based sizing；
3) assembling and pre-connection：1) at least two (such as two) silicon carbide ceramics samples in are passed through at least one (such as one
It is a) joint face connects into a complex, the coated with resins based sizing between silicon carbide ceramics joint face, using mold to connection
Part pressurizes, pressure value 0.5MPa, to improve the stability of connection, then cures at 90,110,130 DEG C respectively
3h removes sample in mold after curing, carries out cracking carbonization at Ar atmosphere, 900 DEG C, obtains pre-connection part；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into pure silicon powder, silicon is controlled by the content of carbon in pre-connection part
The additive amount of powder keeps the temperature the processing of 30min infiltrations at a temperature of 1470 DEG C so that carbon and silicon or siliceous mixture in binder
Reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.By universal testing machine, wherein
Sample is processed into the standard strip of 3mm × 4mm × 36mm, and upper push-down head span is respectively 10mm and 30mm, and loading speed is
0.5mm/min, connection middle layer be maintained at as possible in pressure head away from middle position, obtain jointing three-point bending strength with
And elasticity modulus, and connection layer thickness is measured, it the results are shown in Table 1.
Embodiment 2
1) pre-treatment；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：Phenolic resin 25%, ethyl alcohol 25%, silicon carbide micro-powder 50%；And point of the weight for principal component total amount 5%
Powder polyethylene pyrrole network alkanone, weight are the curing agent hexamethylene tetramine of principal component total amount 4%；
3) assembling and pre-connection：1) at least two (such as two) silicon carbide ceramics samples in are passed through at least one (such as one
It is a) joint face connects into a complex, and coated with resins based sizing, adds connector between silicon carbide ceramics joint face
Pressure, pressure value 0.2MPa to improve the stability of connection, then cure 4h at 80,100,120 DEG C respectively, then exist
Ar atmosphere carries out cracking carbonization at 900 DEG C, obtains pre-connection part；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into powder containing pure silicon, is controlled by the content of carbon in pre-connection part
The additive amount of silica flour keeps the temperature the processing of 15min infiltrations at a temperature of 1500 DEG C so that carbon in binder and silicon siliceous mix
Object reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.It is strong to measure jointing three-point bending
Degree, the elasticity modulus of connector and connection layer thickness, the results are shown in Table 1.
Fig. 1 is that embodiment 2 connects sample joint microstructure morphology scanning electron microscope image, and the right and left is SiC ceramic
Matrix, for articulamentum, wherein white area be the α-SiC phases of addition for centre, light gray areas be the newly-generated β of reaction in-situ-
SiC phases, dark gray areas are free silica, and wherein contents of free si corrodes sample by HF acid front and rear weight difference and calculates, and obtains
Contents of free si is 11%.As shown in Figure 1, connection layer thickness is uniform, at articulamentum and parent material interface the defects of free from flaw, fracture
In the presence of.
Embodiment 3
1) pre-treatment；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：Phenolic resin 30%, ethyl alcohol 30%, silicon carbide micro-powder 35%, carbon black 5%；And weight is principal component total amount
4% polyethylene of dispersing agent pyrrole network alkanone, weight are the curing agent of principal component total amount 4%；
3) assembling and pre-connection：1) at least two (such as two) silicon carbide ceramics samples in are passed through at least one (such as one
It is a) joint face connects into a complex, and coated with resins based sizing, adds connector between silicon carbide ceramics joint face
Pressure, pressure value 0.5MPa to improve the stability of connection, then cure 6h, then in Ar at 70,90,110 DEG C respectively
Atmosphere carries out cracking carbonization at 900 DEG C, obtains pre-connection part；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into pure silicon powder, silicon is controlled by the content of carbon in pre-connection part
The additive amount of powder keeps the temperature the processing of 15min infiltrations at a temperature of 1500 DEG C so that carbon and silicon or siliceous mixture in binder
Reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.It is strong to measure jointing three-point bending
Degree, the elasticity modulus of connector and connection layer thickness, the results are shown in Table 1.
Fig. 2 is that embodiment 3 connects sample joint microstructure morphology scanning electron microscope image, and the right and left is SiC ceramic
Matrix, for articulamentum, wherein white area be the α-SiC phases of addition for centre, light gray areas be the newly-generated β of reaction in-situ-
SiC phases, dark gray areas are free silica, contents of free si 32%.As shown in Figure 2, connection layer thickness is uniform, articulamentum and mother
The defects of material interface free from flaw, fracture, exists.
Embodiment 4
1) pre-treatment；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：Phenolic resin 30%, ethyl alcohol 30%, silicon carbide micro-powder 30%, carbon black 10%；And weight is total for principal component
The dispersant of 4-5% is measured, weight is the curing agent of principal component total amount 4%；
3) assembling and pre-connection：1) at least two (such as two) silicon carbide ceramics samples in are passed through at least one (such as one
It is a) joint face connects into a complex, and coated with resins based sizing, adds connector between silicon carbide ceramics joint face
Pressure, pressure value 0.2MPa to improve the stability of connection, then cure 4h at 80,100,120 DEG C respectively, then exist
Ar atmosphere carries out cracking carbonization at 900 DEG C, obtains pre-connection part；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into siliceous mixture, by the content control of carbon in pre-connection part
The additive amount of silica flour processed keeps the temperature the processing of 15min infiltrations at a temperature of 1500 DEG C so that carbon and silicon or siliceous mixed in binder
Close object reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.Measure jointing three-point bending
Intensity, the elasticity modulus of connector and connection layer thickness, the results are shown in Table 1.
Embodiment 5
1) pre-treatment；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：Furfuryl alcohol resin 30%, ethyl alcohol 30%, silicon carbide micro-powder 40%；And weight is principal component total amount 4-5%'s
Dispersant, weight are the curing agent of principal component total amount 4%；
3) assembling and pre-connection：1) at least two (such as two) silicon carbide ceramics samples in are passed through at least one (such as one
It is a) joint face connects into a complex, and coated with resins based sizing, adds connector between silicon carbide ceramics joint face
Pressure, pressure value 0.5MPa to improve the stability of connection, then cure 4h at 80,100,120 DEG C respectively, then exist
Ar atmosphere carries out cracking carbonization at 900 DEG C, obtains pre-connection part；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into siliceous mixture, includes silica flour 95%, niobium powder 5%；By
The additive amount of the content control silica flour of carbon, keeps the temperature the processing of 15min infiltrations so that connection at a temperature of 1500 DEG C in pre-connection part
Carbon in material reacts generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected with silicon or siliceous mixture.
Jointing three-point bending strength, the elasticity modulus of connector and connection layer thickness are measured, the results are shown in Table 1.
Embodiment 6
1) pre-treatment；
2) resin based sizing is prepared：With embodiment 1；
3) assembling and pre-connection：With embodiment 1；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into pure silicon powder, silicon is controlled by the content of carbon in pre-connection part
The additive amount of powder keeps the temperature the processing of 15min infiltrations at a temperature of 1550 DEG C so that carbon and silicon or siliceous mixture in binder
Reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.It is strong to measure jointing three-point bending
Degree, the elasticity modulus of connector and connection layer thickness, the results are shown in Table 1.
Embodiment 7
1) pre-treatment；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：With embodiment 1；
3) assembling and pre-connection：With embodiment 1；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into pure silicon powder, silicon is controlled by the content of carbon in pre-connection part
The additive amount of powder keeps the temperature the processing of 15min infiltrations at a temperature of 1600 DEG C so that carbon and silicon or siliceous mixture in binder
Reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.It is strong to measure jointing three-point bending
Degree, the elasticity modulus of connector and connection layer thickness, the results are shown in Table 1.
Embodiment 8
1) pre-treatment；
2) resin based sizing is prepared：With embodiment 1；
3) assembling and pre-connection：With embodiment 1；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into siliceous mixture, including silica flour 95%, molybdenum powder 5%, by
The additive amount of the content control silica flour of carbon, keeps the temperature the processing of 15min infiltrations so that connection at a temperature of 1500 DEG C in pre-connection part
Carbon in material reacts generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected with silicon or siliceous mixture.
Jointing three-point bending strength, the elasticity modulus of connector and connection layer thickness are measured, the results are shown in Table 1.
Embodiment 9
1) pre-treatment；
2) resin based sizing is prepared：With embodiment 1；
3) assembling and pre-connection：With embodiment 1；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into siliceous mixture, including silica flour 92%, molybdenum powder 8%, by
The additive amount of the content control silica flour of carbon, keeps the temperature the processing of 15min infiltrations so that connection at a temperature of 1500 DEG C in pre-connection part
Carbon in material reacts generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected with silicon or siliceous mixture.
Jointing three-point bending strength, the elasticity modulus of connector and connection layer thickness are measured, the results are shown in Table 1.
Embodiment 10
1) pre-treatment；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：Phenolic resin 30%, ethyl alcohol 30%, silicon carbide micro-powder 40%；And weight is principal component total amount 4-5%'s
Dispersant, weight are the curing agent of principal component total amount 4%；
3) assembling and pre-connection：1) at least two (such as two) silicon carbide ceramics samples in are passed through at least one (such as one
It is a) joint face connects into a complex, and coated with resins based sizing, adds connector between silicon carbide ceramics joint face
Pressure, pressure value 0.3MPa to improve the stability of connection, then cure 4h at 80,100,120 DEG C respectively, then exist
Ar atmosphere carries out cracking carbonization at 900 DEG C, obtains pre-connection part；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into pure silicon powder, silicon is controlled by the content of carbon in pre-connection part
The additive amount of powder keeps the temperature the processing of 15min infiltrations at a temperature of 1500 DEG C so that carbon and silicon or siliceous mixture in binder
Reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.It is strong to measure jointing three-point bending
Degree, the elasticity modulus of connector and connection layer thickness, the results are shown in Table 1.
Embodiment 11
1) pre-treatment；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：Phenolic resin 30%, ethyl alcohol 30%, silicon carbide micro-powder 40%；And weight is principal component total amount 4-5%'s
Dispersant, weight are the curing agent of principal component total amount 4%；
3) assembling and pre-connection：1) at least two (such as two) silicon carbide ceramics samples in are passed through at least one (such as one
It is a) joint face connects into a complex, and coated with resins based sizing, adds connector between silicon carbide ceramics joint face
Pressure, pressure value 0.2MPa to improve the stability of connection, then cure 4h at 80,100,120 DEG C respectively, then exist
Ar atmosphere carries out cracking carbonization at 900 DEG C, obtains pre-connection part；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into pure silicon powder, silicon is controlled by the content of carbon in pre-connection part
The additive amount of powder keeps the temperature the processing of 15min infiltrations at a temperature of 1500 DEG C so that carbon and silicon or siliceous mixture in binder
Reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.It is strong to measure jointing three-point bending
Degree, the elasticity modulus of connector and connection layer thickness, the results are shown in Table 1.
Embodiment 12
1) pre-treatment；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：Phenolic resin 30%, ethyl alcohol 30%, silicon carbide micro-powder 40%；And weight is principal component total amount 4-5%'s
Dispersant, weight are the curing agent of principal component total amount 4%；
3) assembling and pre-connection：1) at least two (such as two) silicon carbide ceramics samples in are passed through at least one (such as one
It is a) joint face connects into a complex, and coated with resins based sizing, adds connector between silicon carbide ceramics joint face
Pressure, pressure value 0.1MPa to improve the stability of connection, then cure 4h at 80,100,120 DEG C respectively, then exist
Ar atmosphere carries out cracking carbonization at 900 DEG C, obtains pre-connection part；
4) high temperature siliconising reaction forming：Above-mentioned pre-connection part is buried into pure silicon powder, silicon is controlled by the content of carbon in pre-connection part
The additive amount of powder keeps the temperature the processing of 15min infiltrations at a temperature of 1500 DEG C so that carbon and silicon or siliceous mixture in binder
Reaction generation articulamentum, so as to fulfill being stably connected with, the silicon carbide ceramics that is connected.It is strong to measure jointing three-point bending
Degree, the elasticity modulus of connector and connection layer thickness, the results are shown in Table 1.
Table 1 shows the jointing three-point bending strength of embodiment 1-12, the elasticity modulus of connector and connection layer thickness
Test result.
Table 1：
Table 1 is for specific connection example switching performance as a result, table Elastic Modulus and bending strength test are that multiple samples are surveyed
The average value of test result.It can be obtained by data in table, the connection sample strength that this connection method obtains is high, and connection layer thickness is uniform,
It can realize and be stably connected with.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Comparative example 1
1) pre-treatment；
2) slurry is prepared：Prepare raw material according to following proportioning,
Principal component：Graphite powder 60%, ethyl alcohol 40%；
3) it assembles and connects：1) at least two (such as two) silicon carbide ceramics samples in are passed through at least one (such as one)
Joint face connects into a complex, slurry in being coated 2) between silicon carbide ceramics joint face, by clamping mould, 120
Dry 4h at DEG C；Then mold is placed in high temperature furnace, silica flour is placed in sample junction, is kept the temperature at a temperature of 1470 DEG C
15min infiltrations processing so that carbon in binder and silicon react and generates articulamentum, the silicon carbide ceramics connected.Gained
Connector bonding strength is 130 ± 39MPa, and Major Difficulties are mould during the uncontrollable and high temperature siliconising of articulamentum pore structure
The technology difficulty that tool clamping is brought.
Comparative example 2
1) pre-treatment；
2) resin based sizing is prepared：Prepare raw material according to following proportioning,
Principal component：Phenolic resin 37.5%, ethyl alcohol 37.5%, silicon carbide micro-powder 25%；And weight is principal component total amount 4%
Polyethylene of dispersing agent pyrrole network alkanone, weight be principal component total amount 4% curing agent benzene sulfonyl chloride；
3) assembling and pre-connection：With embodiment 1；
4) high temperature siliconising reaction forming：With embodiment 1.Gained connector bonding strength is 40 ± 8MPa, and switching performance is poor, main
If due to silicon carbide micro-powder content it is relatively low when, slurry viscosity is too small, and slurry dispersion stabilization is poor.
Claims (10)
1. a kind of resin based sizing, which is characterized in that the resin based sizing includes：
Weight percentage, resin 25~35%, organic solvent 25~35% and silicon carbide micro-powder 30~50%.
2. resin based sizing according to claim 1, which is characterized in that the resin based sizing further includes 0~10wt%'s
Carbon black.
3. resin based sizing according to claim 1 or 2, which is characterized in that the resin based sizing further includes 4~5
The curing agent of the dispersant of wt%, and/or 2~10 wt%, the dispersant are selected from polyvinylpyrrolidone, polyacrylamide, phosphorus
At least one of hydrochlorate；The curing agent is selected from benzene sulfonyl chloride and/or hexa.
4. resin based sizing according to any one of claim 1 to 3, which is characterized in that the resin is organic carbonaceous
Resin, preferably phenolic resin and/or furfuryl alcohol resin；The organic solvent be alcohols, preferably ethyl alcohol, ethylene glycol, polyethylene glycol,
At least one of diglycol, three contracting triethylene glycols.
A kind of 5. silicon carbide ceramics reaction forming method, which is characterized in that the method is with any one of claims 1 to 4 institute
The resin based sizing stated connects silicon carbide ceramic components for binder, including：
At least two silicon carbide ceramic components are connected into complex by least one joint face, are connected in silicon carbide ceramic components
Resin based sizing any one of Claims 1-4 is coated between junction, cure under pressure, cracking unsticking is carried out, obtains pre-
Connector；
The position that is at least connected with of the pre-connection part is buried into silicon source, melts at a temperature of 1400~1700 DEG C and oozes processing, it is raw
It is connected into articulamentum with realizing.
6. connection method according to claim 5, which is characterized in that the pressure of the pressurization is described in 0.1~0.5MPa
Cured temperature schedule is gradient increased temperature, is preferably warming up to after 70~90 DEG C and starts to keep the temperature, then often increase 20 DEG C of heat preservations 2~
6 hours, until 110~130 DEG C.
7. connection method according to claim 5 or 6, which is characterized in that the cracking unsticking temperature is 900-1200 DEG C,
Heating rate is 1~2.5 DEG C/min.
8. connection method according to any one of claims 5 to 7, which is characterized in that the silicon source at least contains simple substance
Silicon is preferably made of pure silicon or silicon and refractory metal.
9. the connection method according to any one of claim 5 to 8, which is characterized in that described melt oozes time of processing and be
10~30 minutes.
10. the connection method according to any one of claim 5 to 9, which is characterized in that the thickness of the articulamentum is 5
~200 μm.
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| CN113402289A (en) * | 2021-05-08 | 2021-09-17 | 中广核研究院有限公司 | Silicon carbide cladding induction heating connection method and silicon carbide cladding |
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