CN103964884A - Connection method for silicon carbide ceramics - Google Patents
Connection method for silicon carbide ceramics Download PDFInfo
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- CN103964884A CN103964884A CN201310040858.6A CN201310040858A CN103964884A CN 103964884 A CN103964884 A CN 103964884A CN 201310040858 A CN201310040858 A CN 201310040858A CN 103964884 A CN103964884 A CN 103964884A
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Abstract
The invention provides a connection method for silicon carbide ceramics. The method comprises the steps of: (a) providing a ceramic slurry containing silicon carbide ceramic powder; providing a to-be-connected silicon carbide ceramic body, with an assembly tolerance reserved between to-be-connected surfaces of the body; (b) subjecting the to-be-connected surfaces of the body to in situ solidification connection through the ceramic slurry to obtain a connected body; and (c) conducting high temperature sintering on the connected body, thus obtaining a connected silicon carbide ceramic component. The silicon carbide ceramic pipe connection method provided by the invention can realize high strength connection of silicon carbide ceramic pipes and can improve the performance of the overall ceramic component.
Description
Technical field
The present invention relates to a kind of method of attachment of silicon carbide ceramics, relate to or rather a kind of in-situ solidifying and high temperature co-firing method of attachment of silicon carbide ceramics tubing.Belong to engineering ceramic material technical field.
Background technology
Silicon carbide is a kind of important non-oxide ceramic material, there is good hardness, the performance such as high temperature resistant, anti-oxidant, corrosion-resistant, wear-resistant, the sealing member that is widely used in mechanical structural part and chemical field, wearing pieces etc., the silicon carbide ceramics of special normal pressure solid state sintering system is to bring into play irreplaceable effect under the severe condition such as strong acid, highly basic, high wearing and tearing, high temperature.
High temperature resistant and the corrosion resistance nature of silicon carbide ceramics excellence, high thermal conductivity and mechanical strength, the solar heat protection under high temperature and deep-etching condition, heating, heat exchange field have important application prospect.The protecting tube of preparing with silicon carbide ceramics, use temperature can reach 1600 ° of C, and thermal shock resistance is good, can be with the thermometric protection under the severe condition such as corrosion-resistant.The interchanger use temperature of preparing with carborundum heat-exchange tube can reach 1300 ° more than C, can bear harsher environment, and work-ing life is higher more than 3 times than traditional metal interchanger, and heat exchange efficiency also improves greatly.Meanwhile, silicon carbide ceramics also has important application prospect in field of electric heating, can be used in higher heating power, in the interior heating field of strong acid and strong base, has also tentatively presented advantage.
In these application, the encapsulation of silicon carbide ceramics tubing and connection are gordian techniquies.Pottery tubing is generally prepared by isostatic pressing, injection forming and extruding-out process, and wherein the production efficiency of extrusion moulding, yield rate, serialization and level of automation are higher.In actual use, conventionally need to be connected with another ceramic component its one or both ends.The performance of connecting material and the overall performance of ceramic component are closely related, the particularly application in some severe rugged environments, the resistance to elevated temperatures of junction and withstand voltage properties are had higher requirement to ceramic mode of connection and material, are directly connected to the work-ing life of integral unit.
Welding is an important technique, but the performance of scolder, has greatly limited the application of ceramic component under severe condition with thermal mismatching of ceramic matrix etc.Diffusion welding is a kind of more effective ceramic mode of connection, and two interfaces when approaching the heat pottery joint surface of ceramic fusing point are mutually bonding, but this process costs is higher, and needs external pressurized.Meanwhile, under the condition of high temperature, the different butt seams place of thermal expansivity produces pressure, the defect such as easily cracks.Recently adopting ceramic forerunner scolder is a novel method of attachment, by use Production of Ceramics polymkeric substance under certain ceramics processing temperature, realizes the connection of ceramic component, and does not produce the problem that heat coupling is inconsistent and pollute.
Chinese invention patent CN100393509C provides a kind of method of attachment of silicon carbide ceramic components, powder by bimolecular silicon carbide mixes with pottery generation polymkeric substance, form with slurry is exerted pressure, and then heated polymerizable thing cracking is converted to pottery parts are connected.This connection technique can connect the ceramic component of different shape complexity, but owing to not having outside to exert pressure, but bonding strength is not high, and the use properties under severe rugged environment is restricted.
In the connection of ceramic tubing, by base substrate, connecting the technique of then burning is altogether a kind of more effective method of attachment.U.S. patent of invention US4923655, US5112544, US5043116 etc., provided a kind of connection technique of ceramics extrusion molding blank, employing organic foam stops up, the method sealing of slurry dipping, and the through hole base substrate tubing that this technique be take after extrusion moulding carries out end sealer to tubing base substrate as matrix, need size performance and base substrate in full accord, exist the problem that dry shrinkage is inhomogeneous, sintering is easy to crack.
By above analysis, can find out, directly slurry connects ceramic body due to the performance difference of size performance and dry rear base substrate, causes connecting rear ceramic various piece density unevenness one, and inner generation causes material property to decline compared with large stress concentration.And the method for diffusion welding needs outside to exert pressure, need High Temperature High Pressure, equipment and process is complicated.
In sum, at present, ripe technique without comparison aspect the connection with no pressure of ceramic tubing base substrate.
Therefore, this area connects in the urgent need to a kind of high strength that realizes silicon carbide ceramics tubing, improves the silicon carbide ceramics tubing method of attachment of the performance of bulk ceramics parts.
Summary of the invention
The first object of the present invention is to obtain a kind of high strength that realizes silicon carbide ceramics tubing and connects, and improves the silicon carbide ceramics tubing method of attachment of the performance of bulk ceramics parts.
The second object of the present invention is to obtain a kind of high strength that realizes silicon carbide ceramics tubing and connects, the ceramic size that the silicon carbide ceramics tubing of the performance of raising bulk ceramics parts connects.
The 3rd object of the present invention is to obtain a kind of high strength that realizes silicon carbide ceramics tubing and connects, the purposes of the ceramic size that the silicon carbide ceramics tubing of the performance of raising bulk ceramics parts connects.
In a first aspect of the present invention, a kind of method of attachment of silicon carbide ceramics is provided, described method comprises the steps:
(a) provide the ceramic size that contains Silicon Carbide Powder;
Provide silicon carbide ceramic body to be connected, reserved fitting allowance between the surface to be connected of described base substrate;
(b) in-situ solidifying connection is carried out by described ceramic size in the surface to be connected of described base substrate, obtains the base substrate connecting;
(c) base substrate of described connection carries out high temperature sintering, obtains the silicon carbide ceramic components connecting.
In an embodiment, the ceramic component after ceramic blank drying, unsticking after curing connection are connected with high temperature sintering.
In an embodiment, the method comprises slurry preparation, base substrate processing, in-situ solidifying, the steps such as high-temperature heat treatment (seeing accompanying drawing 2): more specifically, comprise the steps:
(1), by ceramic powder, organic precursor, binding agent, dispersion agent, after ball milling, prepare the mixed slurry of certain solid content.
(2) the ceramic tubing base substrate outer face that will connect and another ceramic component bore surface carry out respectively mechanical workout, and reserved certain rigger is poor.
The high temperature sintering volumetric shrinkage of described ceramic tubing base substrate is less than another ceramic component, and difference is 2-5%.
Two described surperficial riggers are poor is 10-30 silk, and optimizing tolerance is 15.
(3) outside surface of tubing base substrate is immersed to ceramic size, static for some time takes out, and is placed to another ceramic component endoporus, solidifies for some time.
(4) ceramic component after ceramic blank drying, unsticking after solidify connecting are connected with high temperature sintering.
In a specific embodiment of the present invention, in step (a),
Described silicon carbide ceramic body to be connected comprises the first silicon carbide ceramic body and the second silicon carbide ceramic body;
The bore surface of the outside surface of described the first silicon carbide ceramic body and the second silicon carbide ceramic body carries out respectively mechanical workout, thereby reserved described rigger is poor.
In an embodiment, the high temperature sintering volumetric shrinkage of ceramic tubing base substrate is less than another ceramic component, and difference is 2-5%.
In an embodiment, the outside surface of the first silicon carbide ceramic body (for example tubing base substrate) is immersed to ceramic size, static for some time takes out, and is placed to the second silicon carbide ceramic body (another ceramic component) endoporus, solidifies for some time.
In a specific embodiment of the present invention, the high temperature sintering volumetric shrinkage of described the first silicon carbide ceramic body is less than described the second silicon carbide ceramic body; Preferably, described difference is 2-5%, with the volume calculating of described the first silicon carbide ceramic body.
In a specific embodiment of the present invention, described fitting allowance is 10-30 silk.
In an embodiment, optimizing tolerance is 15.
A second aspect of the present invention provides a kind of ceramic size connecting for silicon carbide ceramics, and described ceramic size comprises:
The Silicon Carbide Powder of 5～30 weight parts;
The optional silicon oxide of 0～15 weight part;
The silicon carbide precursor body of 5～20 weight parts;
The binding agent of 2～10 weight parts;
The optional dispersion agent of 0～2 weight part;
And the solvent of significant quantity.
Described solvent can be the mixture of toluene or dimethylbenzene and deionized water, and wherein the content of water is 50-80vol%.The former is for dissolving organic precursor.
In a specific embodiment of the present invention, described silicon oxide is Powdered silicon oxide or silicon sol.
In a specific embodiment of the present invention, described silicon carbide precursor body is selected from polymethyl silicane, poly-methyl hydrogen silane, polychloromethylsilane, Polymethylphenylsilane, Polycarbosilane or its combination.
In a specific embodiment of the present invention, described binding agent is resol, polyvinyl alcohol, polyoxyethylene glycol or its mixture.
In a specific embodiment of the present invention, described dispersion agent copper plate ammonium polymethacrylate, sodium polymethacrylate, tetramethyl-oxyammonia or its combination.
The application that a third aspect of the present invention provides a kind of ceramic size of the present invention to connect at silicon carbide ceramics.
Accompanying drawing explanation
The johning knot composition of the typical silicon carbide ceramics tubing of Fig. 1 and another parts.
Fig. 2 method of attachment schema.
Embodiment
The inventor is through extensive and deep research, by improving preparation technology, saving grace in conjunction with existing technique, propose a kind of in-situ solidifying technique and connected ceramic tubing base substrate, the connection technique of high temperature integrated sintering then, for the high strength that realizes silicon carbide ceramics tubing, connect, the performance that improves bulk ceramics parts has good effect.Completed on this basis the present invention.
Technical conceive of the present invention is as follows:
The invention provides a kind of method of attachment of silicon carbide ceramics, belong to engineering ceramic material technical field.It is characterized in that adopting in-situ solidifying technique to connect silicon carbide ceramic body, high temperature integrated sintering connects silicon carbide ceramics.
In addition, the present invention also provides a kind of ceramic size, is mainly applicable to the connection of normal pressure solid-phase sintered silicon carbide ceramics.First by Silicon Carbide Powder, organic precursor, binding agent, dispersion agent is prepared the slurry of certain solid content after ball milling.The ceramic body joint face that will connect is processed respectively, and reserved certain rigger is poor, and surface uniform applies and connects slurry, and after fixing, be dried, unsticking is connected silicon carbide ceramics with high temperature sintering.This connection technique is simple and convenient, is specially adapted to connect ceramic tubing and other structural parts, at ceramic heat exchanger pipe-pipe, pipe-plate, connects, and ceramic tubing sealing connects, and the connection of other complex shape ceramic component has important application prospect.
In the present invention, term " contains " or " comprising " represents that various compositions can be applied in mixture of the present invention or composition together.Therefore, term " mainly by ... form " and " by ... composition " be included in that term " contains " or in " comprising ".
Herein, described " silicon carbide ceramics " comprises the various silicon carbide ceramics in this area.For example, include but not limited to: the silicon carbide ceramics of normal pressure solid state sintering system.
Herein, described " connection of silicon carbide ceramics " includes but not limited to: the heat exchanger tube-pipe of silicon carbide ceramics, pipe-plate connect, and ceramic tubing sealing connects, and the connection of other complex shape ceramic component.
Herein, described " high temperature sintering " has the conventional sense of this area.Conventionally, described high temperature includes but not limited to 1800-2200 ℃.
Below describe in detail to various aspects of the present invention:
The method of attachment of silicon carbide ceramics
In a first aspect of the present invention, a kind of method of attachment of silicon carbide ceramics is provided, described method comprises the steps:
(a) provide the ceramic size that contains Silicon Carbide Powder;
Provide silicon carbide ceramic body to be connected, reserved fitting allowance between the surface to be connected of described base substrate;
(b) in-situ solidifying connection is carried out by described ceramic size in the surface to be connected of described base substrate, obtains the base substrate connecting;
(c) base substrate of described connection carries out high temperature sintering, obtains the silicon carbide ceramic components connecting.
In an embodiment, the ceramic component after ceramic blank drying, unsticking after curing connection are connected with high temperature sintering.
The inventor connects silicon carbide ceramic body by in-situ solidifying technique, and high temperature integrated sintering connects silicon carbide ceramics, and the high strength that realizes silicon carbide ceramics tubing connects, and improves the performance of bulk ceramics parts.
In an embodiment, the method comprises slurry preparation, base substrate processing, in-situ solidifying, the steps such as high-temperature heat treatment (seeing accompanying drawing 2): more specifically, comprise the steps:
(1), by ceramic powder, organic precursor, binding agent, dispersion agent, after ball milling, prepare the mixed slurry of certain solid content.
(2) the ceramic tubing base substrate outer face that will connect and another ceramic component bore surface carry out respectively mechanical workout, and reserved certain rigger is poor.
The high temperature sintering volumetric shrinkage of described ceramic tubing base substrate is less than another ceramic component, and difference is 2-5%.
Two described surperficial riggers are poor is 10-30 silk, and optimizing tolerance is 15.
(3) outside surface of tubing base substrate is immersed to ceramic size, static for some time takes out, and is placed to another ceramic component endoporus, solidifies for some time.
(4) ceramic component after ceramic blank drying, unsticking after solidify connecting are connected with high temperature sintering.
In a specific embodiment of the present invention, in step (a),
Described silicon carbide ceramic body to be connected comprises the first silicon carbide ceramic body and the second silicon carbide ceramic body;
The bore surface of the outside surface of described the first silicon carbide ceramic body and the second silicon carbide ceramic body carries out respectively mechanical workout, thereby reserved described rigger is poor.
In an embodiment, the high temperature sintering volumetric shrinkage of ceramic tubing base substrate is less than another ceramic component, and difference is 2-5%.
In an embodiment, the outside surface of the first silicon carbide ceramic body (for example tubing base substrate) is immersed to ceramic size, static for some time takes out, and is placed to the second silicon carbide ceramic body (another ceramic component) endoporus, solidifies for some time.
In a specific embodiment of the present invention, the high temperature sintering volumetric shrinkage of described the first silicon carbide ceramic body is less than described the second silicon carbide ceramic body; Preferably, described difference is 2-5%, with the volume calculating of described the first silicon carbide ceramic body.
In a specific embodiment of the present invention, described fitting allowance is 10-30 silk.
In an embodiment, optimizing tolerance is 15.
The ceramic size that silicon carbide ceramics connects
A second aspect of the present invention provides a kind of ceramic size connecting for silicon carbide ceramics, and described ceramic size comprises:
The Silicon Carbide Powder of 5～30 weight parts; Preferred 10-25 weight part
The optional silicon oxide of 0～15 weight part; Preferred 3-10 weight part
The silicon carbide precursor body of 5～20 weight parts; Preferred 10-15 weight part
The binding agent of 2～10 weight parts; Preferred 3-6 weight part
The optional dispersion agent of 0～2 weight part; Preferred 0～1.0 weight part
And the solvent of significant quantity.
Conventionally, described silicon carbide precursor body is organic precursor.In a specific embodiment of the present invention, described silicon carbide precursor body is selected from polymethyl silicane, poly-methyl hydrogen silane, polychloromethylsilane, Polymethylphenylsilane, Polycarbosilane or its combination.
Described " significant quantity " refers to, can dissolve the consumption of described silicon carbide precursor body.The silicon carbide precursor body that described solvent-soluble solution is used, is not specifically limited.For example, can be the mixture of toluene or dimethylbenzene and deionized water, wherein the content of water is 50-80vol%.
In a specific embodiment of the present invention, described silicon oxide is Powdered silicon oxide or silicon sol.
In an embodiment, in described ceramic size, wrap ceramic powder, organic precursor, binding agent, dispersion agent and solvent etc., be prepared from through clipping the ball mill.
In an embodiment, described ceramic powder comprises silicon carbide and silicon oxide.Wherein the content of silicon carbide is 5-30wt%, and optimization content is 10-25wt%.Silicon oxide can be Powdered, can be also equivalent silicon sol, and its content is at 0-15wt%, and optimization content is 3-10wt%.
In an embodiment, described organic precursor can be polymethyl silicane, poly-methyl hydrogen silane, polychloromethylsilane, Polymethylphenylsilane, the presoma of the silicon carbide such as Polycarbosilane, its content can be 5-20wt%, and optimization content is 10-15wt%.
In an embodiment, described binding agent can be resol, polyvinyl alcohol, and polyoxyethylene glycol or its mixture, its content can 2-10wt%, and optimization content is 3-6wt%.
In an embodiment, described dispersion agent can be ammonium polymethacrylate, sodium polymethacrylate or tetramethyl-oxyammonia etc., and its content can be 0～2wt%, and optimization content is 0～1.0wt%.
In a specific embodiment of the present invention, described binding agent is resol, polyvinyl alcohol, polyoxyethylene glycol or its mixture.
In a specific embodiment of the present invention, described dispersion agent is selected from ammonium polymethacrylate, sodium polymethacrylate, tetramethyl-oxyammonia or its combination.
The invention has the advantages that, a kind of method of attachment of silicon carbide ceramics is provided, belong to engineering ceramic material technical field.It is characterized in that adopting in-situ solidifying technique to connect silicon carbide ceramic body, high temperature integrated sintering connects silicon carbide ceramics.In addition, the present invention also provides a kind of ceramic size, is mainly applicable to the connection of normal pressure solid-phase sintered silicon carbide ceramics.First by Silicon Carbide Powder, organic precursor, binding agent, dispersion agent is prepared the slurry of certain solid content after ball milling.The ceramic body joint face that will connect is processed respectively, and reserved certain rigger is poor, and surface uniform applies and connects slurry, and after fixing, be dried, unsticking is connected silicon carbide ceramics with high temperature sintering.This connection technique is simple and convenient, is specially adapted to connect ceramic tubing and other structural parts, at ceramic heat exchanger pipe-pipe, pipe-plate, connects, and ceramic tubing sealing connects, and the connection of other complex shape ceramic component has important application prospect.
The preferred embodiment of the present invention
The present invention also provides a kind of preferred method of attachment of silicon carbide ceramics.Specifically refer to being connected of a kind of ceramic body tubing and another ceramic component, by two kinds of ceramic components of ceramic size in-situ solidifying, wherein the design high temperature sintering shrinkage ratio of external ceramic parts pottery tubing shrinking percentage is high, in high-temperature sintering process, progressively contact surface is exerted pressure, simultaneously ceramic size component and silicon carbide ceramics generation solid state reaction, thus realize the connection of two ceramic components.The syndeton of typical silicon carbide ceramics tubing and another parts is shown in accompanying drawing 1.
Method of attachment of the present invention realizes by following method, and the method comprises slurry preparation, base substrate processing, and in-situ solidifying, the steps such as high-temperature heat treatment (seeing accompanying drawing 2):
(1), by ceramic powder, organic precursor, binding agent, dispersion agent, after ball milling, prepare the mixed slurry of certain solid content.
(2) the ceramic tubing base substrate outer face that will connect and another ceramic component bore surface carry out respectively mechanical workout, and reserved certain rigger is poor.
The high temperature sintering volumetric shrinkage of described ceramic tubing base substrate is less than another ceramic component, and difference is 2-5%.
Two described surperficial riggers are poor is 10-30 silk, and optimizing tolerance is 15.
(3) outside surface of tubing base substrate is immersed to ceramic size, static for some time takes out, and is placed to another ceramic component endoporus, solidifies for some time.
(4) ceramic component after ceramic blank drying, unsticking after solidify connecting are connected with high temperature sintering.
The present invention also provides a kind of ceramic size that connects normal pressure solid-phase sintered silicon carbide ceramics:
In described ceramic size, wrap ceramic powder, organic precursor, binding agent, dispersion agent and solvent etc., be prepared from through clipping the ball mill.
Described ceramic powder comprises silicon carbide and silicon oxide.Wherein the content of silicon carbide is 5-30wt%, and optimization content is 10-25wt%.Silicon oxide can be Powdered, can be also equivalent silicon sol, and its content is at 0-15wt%, and optimization content is 3-10wt%.
Described organic precursor can be polymethyl silicane, poly-methyl hydrogen silane, and polychloromethylsilane, Polymethylphenylsilane, the presoma of the silicon carbide such as Polycarbosilane, its content can be 5-20wt%, optimization content is 10-15wt%.
Described binding agent can be resol, polyvinyl alcohol, and polyoxyethylene glycol or its mixture, its content can 2-10wt%, and optimization content is 3-6wt%.
Described dispersion agent can be ammonium polymethacrylate, sodium polymethacrylate or tetramethyl-oxyammonia etc., and its content can be 0～2wt%, and optimization content is 0～1.0wt%.
Described solvent can be the mixture of toluene or dimethylbenzene and deionized water, and wherein the content of water is 50-80vol%.The former is for dissolving organic precursor.
With existing silicon carbide ceramics method of attachment comparison, the present invention has following advantage:
(1) this mode of connection, not by means of impressed pressure, reacts but form local pressure and high-temperature interface at linkage interface place by different shrinking percentages in high-temperature sintering process the connection that realizes silicon carbide ceramics tubing, and strength of joint is higher.(2) preparation method of the connection slurry adopting is simple, easy to operate.
As no specific instructions, various raw material of the present invention all can obtain by commercially available; Or prepare according to the ordinary method of this area.Unless otherwise defined or described herein, the familiar same meaning of all specialties used herein and scientific words and those skilled in the art.In addition any method similar or impartial to described content and material all can be applicable in the inventive method.
Other aspects of the present invention, due to disclosure herein, are apparent to those skilled in the art.
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.The experimental technique of unreceipted actual conditions in the following example, measures according to national standard conventionally.If there is no corresponding national standard, according to general international standard, normal condition or the condition of advising according to manufacturer, carry out.Unless otherwise indicated, otherwise all umbers are weight part, and all per-cents are weight percentage, and described polymericular weight is number-average molecular weight.
Unless otherwise defined or described herein, the familiar same meaning of all specialties used herein and scientific words and those skilled in the art.In addition any method similar or impartial to described content and material all can be applicable in the inventive method.
The present invention further illustrates embodiment and effect with following non-limiting example:
Embodiment 1
The present embodiment is connected to silicon carbide ceramics tubing on silicon carbide ceramics tube sheet, and the high strength that realizes pipe-plate connects.First by silicon carbide ceramics tubing end face and Excircle machining, tube sheet internal diameter is processed, and making tube outer diameter and tube sheet internal diameter fitting allowance is 10.The about 2%T.D of shrinking percentage difference of the high temperature sintering shrinking percentage of silicon carbide ceramics tubing and tube sheet wherein.Then preparing ceramic size, is 5wt% by carborundum powder body burden, and silica powder body burden is 3wt%, polymethyl silicane content is 10wt%, and phenolic resin content is 3wt%, and ammonium polymethacrylate content is 0.4wt%, toluene and water are mixed solvent, and wherein water-content is 50vol%.After mixing, high-speed stirring is even.Silicon carbide ceramics connecting end surface is immersed to slurry, after assembling, strike off unnecessary slurry.After tubing after connection and tube sheet dry solidification, successful connection after unsticking high temperature co-firing.Pipe-plate linkage interface is clear, does not find any crackle.
The compressive strength of described junction characterizes with resistance to hydrostatic pressure power, and described resistance to hydrostatic pressure power is not less than 6MPa.
Embodiment 2
The present embodiment is connected to silicon carbide ceramics tubing on silicon carbide ceramics tube sheet, and the high strength that realizes pipe-plate connects.First by silicon carbide ceramics tubing end face and Excircle machining, tube sheet internal diameter is processed, and making tube outer diameter and tube sheet internal diameter fitting allowance is 15.The about 5%T.D of shrinking percentage difference of the high temperature sintering shrinking percentage of silicon carbide ceramics tubing and tube sheet wherein.Then prepare ceramic size, by carborundum powder body burden, be 25wt%, in silicon sol, silica powder body burden is 10wt%, poly-methyl hydrogen silane contents is 12wt%, polyvinyl alcohol content is 4wt%, sodium polymethacrylate content is 0.6wt%, and dimethylbenzene and water are mixed solvent, and wherein water-content is 60vol%.After mixing, high-speed stirring is even.Silicon carbide ceramics connecting end surface is immersed to slurry, after assembling, strike off unnecessary slurry.After tubing after connection and tube sheet dry solidification, successful connection after unsticking high temperature co-firing.Tubing linkage interface is clear, does not find any crackle.
The compressive strength of described junction characterizes with resistance to hydrostatic pressure power, and described resistance to hydrostatic pressure power is not less than 6MPa.
Embodiment 3
The present embodiment is by silicon carbide ceramics tubing by telescopic joint to other silicon carbide ceramics tubing, and the high strength that realizes pipe-pipe connects.Two sections of silicon carbide ceramics tubing end faces that first will connect and Excircle machining, casing inner diameter processing, making tube outer diameter and casing inner diameter fitting allowance is 20.The about 3%T.D of shrinking percentage difference of the high temperature sintering shrinking percentage of silicon carbide ceramics tubing and tube sheet wherein.Then preparing ceramic size, is 20wt% by carborundum powder body burden, and silica powder body burden is 6wt%, polychloromethylsilane content is 12wt%, and polyethyleneglycol content is 4wt%, and tetramethyl-oxyammonia content is 0.6wt%, toluene and water are mixed solvent, and wherein water-content is 60vol%.After mixing, high-speed stirring is even.Silicon carbide ceramics connecting end surface is immersed to slurry, after assembling, strike off unnecessary slurry.After tubing after connection and tube sheet dry solidification, successful connection after unsticking high temperature co-firing.Tubing linkage interface is clear, does not find any crackle.
The compressive strength of described junction characterizes with resistance to hydrostatic pressure power, and described resistance to hydrostatic pressure power is not less than 6MPa.
Embodiment 4
The present embodiment is by silicon carbide ceramics tubing by telescopic joint to other silicon carbide ceramics tubing, and the high strength that realizes pipe-pipe connects.Two sections of silicon carbide ceramics tubing end faces that first will connect and Excircle machining, casing inner diameter processing, making tube outer diameter and casing inner diameter fitting allowance is 30.The about 5%T.D of shrinking percentage difference of the high temperature sintering shrinking percentage of silicon carbide ceramics tubing and tube sheet wherein.Then prepare ceramic size, by carborundum powder body burden, be 15wt%, in silicon sol, silica powder body burden is 10wt%, Polymethylphenylsilane content is 15wt%, resol and polyoxyethylene glycol mixture content are 4wt%, ammonium polymethacrylate is 0.6wt%, and dimethylbenzene and water are mixed solvent, and wherein water-content is 60vol%.After mixing, high-speed stirring is even.Silicon carbide ceramics connecting end surface is immersed to slurry, after assembling, strike off unnecessary slurry.After tubing after connection and tube sheet dry solidification, successful connection after unsticking high temperature co-firing.Tubing linkage interface is clear, does not find any crackle.
The compressive strength of described junction characterizes with resistance to hydrostatic pressure power, and described resistance to hydrostatic pressure power is not less than 6MPa.
Embodiment 5
The present embodiment connects silicon carbide ceramics tubing one end by termination, realize the high-intensity sealing of tubing.Silicon carbide ceramics tubing end face and the Excircle machining that first will connect, the processing of termination internal diameter, making tube outer diameter and termination internal diameter fitting allowance is 20.The about 2%T.D of shrinking percentage difference of the high temperature sintering shrinking percentage of silicon carbide ceramics tubing and tube sheet wherein.Then preparing ceramic size, is 15wt% by carborundum powder body burden, and silica powder body burden is 10wt%, Polycarbosilane content is 8wt%, and phenolic resin content is 4wt%, and sodium polymethacrylate content is 1.0wt%, toluene and water are mixed solvent, and wherein water-content is 80vol%.After mixing, high-speed stirring is even.Silicon carbide ceramics connecting end surface is immersed to slurry, after assembling, strike off unnecessary slurry.After tubing after connection and tube sheet dry solidification, successful connection after unsticking high temperature co-firing.Tubing linkage interface is clear, does not find any crackle.
The compressive strength of described junction characterizes with resistance to hydrostatic pressure power, and described resistance to hydrostatic pressure power is not less than 6MPa.
Embodiment 6
The present embodiment connects silicon carbide ceramics tubing one end by termination, realize the high-intensity sealing of tubing.Silicon carbide ceramics tubing end face and the Excircle machining that first will connect, the processing of termination internal diameter, making tube outer diameter and termination internal diameter fitting allowance is 30.The about 3%T.D of shrinking percentage difference of the high temperature sintering shrinking percentage of silicon carbide ceramics tubing and tube sheet wherein.Then prepare ceramic size, by carborundum powder body burden, be 30wt%, in silicon sol, silica powder body burden is 15wt%, Polycarbosilane content is 12wt%, resol and polyvinyl alcohol mixing content are 6wt%, tetramethyl-oxyammonia content is 1.0wt%, and dimethylbenzene and water are mixed solvent, and wherein water-content is 80vol%.After mixing, high-speed stirring is even.Silicon carbide ceramics connecting end surface is immersed to slurry, after assembling, strike off unnecessary slurry.After tubing after connection and tube sheet dry solidification, successful connection after unsticking high temperature co-firing.Tubing linkage interface is clear, does not find any crackle.
The compressive strength of described junction characterizes with resistance to hydrostatic pressure power, and described resistance to hydrostatic pressure power is not less than 6MPa.
The foregoing is only preferred embodiment of the present invention, not in order to limit essence technology contents scope of the present invention, essence technology contents of the present invention is to be broadly defined in the claim scope of application, any technology entity or method that other people complete, if defined identical with the claim scope of application, also or a kind of change of equivalence, all will be regarded as being covered by among this claim scope.
All documents of mentioning in the present invention are all quoted as a reference in this application, just as each piece of document, are quoted as a reference separately.In addition should be understood that, after having read foregoing of the present invention, those skilled in the art can make various changes or modifications the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (10)
1. a method of attachment for silicon carbide ceramics, is characterized in that, described method comprises the steps:
(a) provide the ceramic size that contains Silicon Carbide Powder;
Provide silicon carbide ceramic body to be connected, reserved fitting allowance between the surface to be connected of described base substrate;
(b) in-situ solidifying connection is carried out by described ceramic size in the surface to be connected of described base substrate, obtains the base substrate connecting;
(c) base substrate of described connection carries out high temperature sintering, obtains the silicon carbide ceramic components connecting.
2. the method for claim 1, is characterized in that, in step (a),
Described silicon carbide ceramic body to be connected comprises the first silicon carbide ceramic body and the second silicon carbide ceramic body;
The bore surface of the outside surface of described the first silicon carbide ceramic body and the second silicon carbide ceramic body carries out respectively mechanical workout, thereby reserved described rigger is poor.
3. the method for claim 1, is characterized in that, the high temperature sintering volumetric shrinkage of described the first silicon carbide ceramic body is less than described the second silicon carbide ceramic body; Preferably, described difference is 2-5%, with the volume calculating of described the first silicon carbide ceramic body.
4. the method for claim 1, is characterized in that, described fitting allowance is 10-30 silk.
5. the ceramic size connecting for silicon carbide ceramics, is characterized in that, described ceramic size comprises:
The Silicon Carbide Powder of 5～30 weight parts;
The optional silicon oxide of 0～15 weight part;
The silicon carbide precursor body of 5～20 weight parts;
The binding agent of 2～10 weight parts;
The optional dispersion agent of 0～2 weight part;
And the solvent of significant quantity.
6. ceramic size as claimed in claim 5, is characterized in that, described silicon oxide is Powdered silicon oxide or silicon sol.
7. ceramic size as claimed in claim 5, is characterized in that, described silicon carbide precursor body is selected from polymethyl silicane, poly-methyl hydrogen silane, polychloromethylsilane, Polymethylphenylsilane, Polycarbosilane or its combination.
8. ceramic size as claimed in claim 5, is characterized in that, described binding agent is resol, polyvinyl alcohol, polyoxyethylene glycol or its mixture.
9. ceramic size as claimed in claim 5, is characterized in that, described dispersion agent copper plate ammonium polymethacrylate, sodium polymethacrylate, tetramethyl-oxyammonia or its combination.
10. the application that ceramic size as claimed in claim 5 connects at silicon carbide ceramics.
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