CN104496511B - A kind of online reaction forming method of ceramic form - Google Patents
A kind of online reaction forming method of ceramic form Download PDFInfo
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- CN104496511B CN104496511B CN201410745840.0A CN201410745840A CN104496511B CN 104496511 B CN104496511 B CN 104496511B CN 201410745840 A CN201410745840 A CN 201410745840A CN 104496511 B CN104496511 B CN 104496511B
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Abstract
The invention discloses a kind of online reaction forming method of ceramic form, comprise the following steps: 1) prepare at least two ceramic forms be made up of carbonaceous material respectively; 2) binding agent is prepared; 3) at least two ceramic forms are connected into a complex body by least one joint face, coated with adhesive between the joint face of ceramic form, is then cured; 4) the complex body infiltration reaction after solidification is formed ceramic component.Ceramic form connection method of the present invention reduces difficulty of processing, simplifies operation, and primary first-order equation sintering can realize connection and the densification of base substrate simultaneously, cost-saved, and junction is consistent with the structure properties of mother metal, the precision of final material and good uniformity.
Description
Technical field
The present invention relates to stupalith field, particularly a kind of online reaction forming method of ceramic form.
Background technology
Stupalith is high temperature resistant, corrosion-resistant, wear-resistant and there is different functional performances and be widely used in the fields such as machinery, chemical industry, electronics, aerospace, more and more come into one's own at present.Due to stupalith fragility, hardness is high and impact toughness is low, thus its poor processability, the component manufacturing big-size complicated shape are comparatively difficult, usually need to form by the interconnection technique between pottery or with metallic substance the component that composite structure produces complicated shape.
The main method connected for stupalith at present has soldering, diffusion welding and reaction forming etc.Need before soldering to be carried out by joint face grinding or even polishing smoothing processing, need add certain pressure during welding, impel joint face to carry out metallurgical reaction and solder permeates in pottery, the active solder of fusing is wetting to be connected ceramic component thus forms joint.The main deficiency of brazing pottery be the intensity of brazed joint lower than mother metal, produce stress etc. because the thermal expansivity of foreign material does not mate in joint.Face of weld during diffusion welding stupalith, interlayer surfaces all needs polished finish, needs higher pressure, make ceramic joining face and middle layer close contact during welding, the atom phase mutual diffusion between contact surface thus form firmly joint.It is high to there is Bonding pressure in diffusion welding interconnection technique, and component is yielding, the shortcoming such as can not evenly to exert pressure to complex component.Brazing and diffusion welding all needs to carry out the complicated course of processing to mother metal, and articulamentum is all metal alloy, and performance can not match with mother metal, and the homogeneity of material is poor.
Reaction forming method grows up from SiC reaction is shaped, and is mainly used at present connecting SiC ceramic and fibre-reinforced matrix material.The unique distinction of reaction shaping method of attachment is the design by joint interface composition and structure, make its performance such as mechanics, calorifics very close to the performance being connected mother metal, and the temperature of reaction forming technique is relatively low, technique does not simply need high temperature jig to the parts that are installed.One is studied more successful reaction forming technology is ARCJoinT (Affordable, RobustCeramicJoiningTechnology) technique, and it is the new ceramics interconnection technique succeeded in developing by the Lewis research centre of U.S. NASA.Successfully connect sintered sic, reaction-sintering SIC by this technique, there is high temperature conjunction intensity the highest so far.This technological process is: first carbonaceous mixture is placed into region to be connected, these carbonaceous mixture fixtures are fixed, 10 ~ 20min is solidified at 100 ~ 120 DEG C of temperature, web member is solidified togather, silicon or silicon alloy with sheet, the form of paste or pulpous state is put into around joining zone, then according to the type of impregnant, between 1250 ~ 1425 DEG C of temperature, it heated and be incubated 10 ~ 15min, melting silicon or silicon-refractory metal alloy and carbon react, form the silicon carbide with silicon controlled rectifier content, and other phase composition can be determined according to alloy ingredient.The thickness of contact is adjusted with the clamp pressure provided by the performance regulating carbonaceous mixture.
This reaction forming technique is the connection to RB-SiC pottery, needs to carry out polished finish to the joint face of silicon carbide ceramics, and therefore the difficulty of processing of joint face is large.May cause the contraction occurring ununiformity in final material and undesirably occur in siliconising process, and siliconising process repeats, this can increase material manufacturing cost undoubtedly.
Summary of the invention
The object of the embodiment of the present invention is the defect for above-mentioned prior art, provides a kind of junction consistent with the structure properties of mother metal, the precision of material and the online reaction forming method of the ceramic form of good uniformity.
The technical scheme that the present invention takes to achieve these goals is:
A kind of online reaction forming method of ceramic form, comprises the following steps:
1) at least two ceramic forms be made up of carbonaceous material are respectively prepared;
2) prepare binding agent, described binding agent comprises the component of following weight percentage:
Water 25-35%, polyacrylamide 5-7%, tackiness agent 1-2%, silicon carbide micro-powder 30-45%, silica flour 10-20%, carbon dust 5-8%;
A, polyacrylamide to be added to the water, to stir and make it abundant dissolving, then add tackiness agent, configuration polyacrylamide solution;
B, silica flour, carbon dust and silicon carbide micro-powder to be added in polyacrylamide solution successively, be configured to slip;
C, then ball milling is carried out to slip, obtain binding agent;
3) at least two ceramic forms are connected into a complex body by least one joint face, coated with adhesive between the joint face of ceramic form, is then cured, dry after solidification, obtains composite body;
4) the composite body infiltration reaction after solidification is formed ceramic component.
Described infiltration reaction is included on the joint face between ceramic form and ceramic form and places silicon or silicon alloy, then by placing composite body siliconising process at the temperature of 1350 DEG C-1700 DEG C of silicon or silicon alloy, the bulk ceramics parts making the carbon in ceramic form and binding agent and silicon reaction in－situ generate silicon B-carbide to be combined.
The time of described siliconising process is 1-3 hour.
Described binding agent comprises the component of following weight percentage:
Water 35%, polyacrylamide 7%, tackiness agent 2%, silicon carbide micro-powder 30%, silica flour 20%, carbon dust 6%.
Described silicon carbide micro-powder comprises the silicon carbide micro-powder of the first granularity and the silicon carbide micro-powder of the second granularity, the granularity of the silicon carbide micro-powder of described first granularity is 1-10 μm, the granularity of the silicon carbide micro-powder of described second granularity is 20-40 μm, and the mass ratio of the silicon carbide micro-powder of described first granularity and the silicon carbide micro-powder of described second granularity is 1-2:1.
Described solidification is at room temperature carried out, and described drying comprises places the ceramic form after bonding in an oven, and the temperature of described drying is 110-130 DEG C, and the dry time is 3-5 hour.
Further, also comprise:
After coated with adhesive, joint face is pressurizeed between the joint face of ceramic form, or aim at when using frock to form connecting sewing to the ceramic body connected between joint face, then use binding agent to fill connecting sewing, finally the ceramic form connected is cured.
Described step 1) comprising: utilize existing silicon carbide ceramics gel casting technology, the carbon containing ceramic blank needed for preparation;
Ceramic form is processed, utilizes numerical control machining center, adopt diamond cutter to process single silicon carbide ceramics blank;
Finally utilize binding agent, the above-mentioned ceramic form processed is connected into the composite body with hollow structure.
The time of described ball milling is 15-25 hour.
The beneficial effect that the technical scheme that the embodiment of the present invention provides is brought is:
Ceramic form connection method of the present invention reduces difficulty of processing, simplify operation, connection and the densification of base substrate can be realized by infiltration reaction sintering simultaneously, cost-saved, and junction is consistent with the structure properties of mother metal, the precision of final material and good uniformity.
Accompanying drawing explanation
Fig. 1 is the syndeton schematic diagram of the ceramic form that the embodiment of the present invention provides;
Fig. 2 is the structural representation of the ceramic form of the hollow structure that the embodiment of the present invention provides.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly, below in conjunction with accompanying drawing, embodiment of the present invention is described further in detail.
See Fig. 1, connected by joint face 2 between two ceramic forms 1, ceramic form 1 and joint face 2 are provided with silicon or silicon alloy 3, composite body is siliconising process at the temperature of 1350 DEG C to 1700 DEG C, the compound making the carbon in blank 1 and binding agent 2 and silicon reaction in－situ generate silicon B-carbide to combine, the bulk ceramics parts that structure is consistent.
Embodiment 1
A kind of online reaction forming method of ceramic form, comprises the following steps:
1) two ceramic forms be made up of carbonaceous material are respectively prepared;
2) binding agent is prepared:
A, prepare raw material according to following proportioning:
Water 31.34%, polyacrylamide 6.07%, polyvinylpyrrolidone 1.48%, silicon carbide micro-powder 38.43%, silica flour 15.95%, carbon dust 6.76%.Wherein, the mass ratio of granularity to be the silicon carbide micro-powder of 5 μm and granularity be 30 μm of silicon carbide micro-powders is 1.5:1; Such proportioning can realize good accumulation.
B, polyacrylamide to be added to the water, to stir and make it abundant dissolving, then add polyvinylpyrrolidone, configuration polyacrylamide solution;
C, silica flour, carbon dust and silicon carbide micro-powder to be added in polyacrylamide solution successively, be configured to slip;
D, then ball milling is carried out 20 hours to slip, obtain binding agent;
3) two ceramic forms are connected into a complex body by a joint face, coated with adhesive between the joint face of ceramic form, then self-vulcanizing is carried out, also can pressurize to joint face after coated with adhesive, to improve the stability of joint face, aim at when frock also can be used to form connecting sewing to the base substrate connected between joint face, then binding agent is used to fill connecting sewing, finally it is cured, like this can accurately control linkage seam size, 120 DEG C of dryings in an oven 4 hours are placed after solidification, obtain composite body,
4) by the composite body infiltration reaction after solidification, namely the joint face between ceramic form and ceramic form is placed silicon or silicon alloy, the placement amount of silicon or silicon alloy decides according to the carbon content in ceramic form, siliconising process 2 hours at the temperature of 1650 DEG C, the compound making the carbon in ceramic form and binding agent and silicon reaction in－situ generate silicon B-carbide to combine, the bulk ceramics parts that structure is consistent.
Embodiment 2
Substantially the same manner as Example 1, difference is:
Step 2) prepare in binding agent:
A, prepare raw material according to following proportioning:
Water 25%, polyacrylamide 5%, polyvinyl alcohol 1%, silicon carbide micro-powder 45%, silica flour 16%, carbon dust 8%.Wherein, the mass ratio of granularity to be the silicon carbide micro-powder of 10 μm and granularity be 40 μm of silicon carbide micro-powders is 2:1; The time of ball milling is 15 hours;
Step 3) in place in baking oven 110 DEG C of dryings 5 hours;
Step 4) in siliconising process 3 hours at the temperature of 1350 DEG C.
Embodiment 3
Substantially the same manner as Example 1, difference is:
Step 2) prepare in binding agent:
A, prepare raw material according to following proportioning:
Water 35%, polyacrylamide 7%, polyvinylpyrrolidone 2%, silicon carbide micro-powder 30%, silica flour 20%, carbon dust 6%.
Wherein, the mass ratio of granularity to be the silicon carbide micro-powder of 1 μm and granularity be 20 μm of silicon carbide micro-powders is 1:1; The time of ball milling is 20 hours.
Step 3) in place in baking oven 130 DEG C of dryings 3 hours;
Step 4) in siliconising process 1 hour at the temperature of 1700 DEG C.
Embodiment 4
Substantially the same manner as Example 1, difference is:
Step 2) prepare in binding agent:
A, prepare raw material according to following proportioning:
Water 34.4%, polyacrylamide 6%, polyvinylpyrrolidone 1.5%, silicon carbide micro-powder 43%, silica flour 10%, carbon dust 5%.A kind of particle diameter is used to be the silicon carbide micro-powder of 30 μm, ball milling 15 hours;
Step 3) in place in baking oven 115 DEG C of dryings 3.5 hours;
Step 4) in siliconising process 1.5 hours at the temperature of 1400 DEG C.
The present invention efficiently solves the performance unhomogeneity of ceramic joining region and mother metal, reduces the difficulty of processing of connected piece, decreases ununiformity and not expected problem that repetition infiltration process brings parts.Multiple component can be combined into complex component production size in a straightforward manner comparatively large and there are the parts of the complicated shapes such as hollow, simplify preparation technology, reduce cost.
Adopt Conventional silicon carbide ceramic preparation technique, and existing ceramic joining technique, be difficult to prepare there is hollow structure and the homogeneous ceramic component of performance, adopt the present invention can realize the reliable preparation of these parts.
A kind of preparation method of hollow structure silicon carbide ceramic components:
1) existing silicon carbide ceramics gel casting technology is utilized, the carbon containing ceramic blank needed for preparation,
2) ceramic form processing, utilizes numerical control machining center, adopts diamond cutter to process single silicon carbide ceramics blank;
3) utilize binding agent of the present invention, i.e. vitrified bond, the above-mentioned ceramic form processed is connected into the composite component with hollow structure, then carries out self-vulcanizing, place in baking oven after solidification, 115 DEG C of dryings 4 hours, obtain composite body;
4) composite body places silicon, then the composite body placing silicon is implemented silicon process 2 hours at the temperature of 1550 DEG C, silicon at high temperature melting is infiltrated in composite preform, obtains silicon carbide ceramic product as shown in Figure 2, the through hole 5 of the hollow structure of formation is had in the middle of the base substrate 4 of ceramic form
According to the preparation method of hollow structure silicon carbide ceramic components of the present invention, the silicon carbide ceramic components of any hollow structure can be prepared, be not limited to the hollow structure shown in Fig. 2 provided by the invention, its size also can adjust as required, can obtain large-sized hollow product.Binding agent of the present invention is consistent with mother metal structure properties, has high level of homogeneity.Technique of the present invention is simple, cost-saving; The present invention adopts ceramic form to connect, and joint face processing is simple, and adopts an infiltration reaction sintering, and final component capabilities is homogeneous, does not have local contraction, does not have stress.Comparatively prior art integrated artistic is simple, cost-saving.
The present invention's parts to be produced are that the blank combination be made up of multiple carbon-containing composite material becomes a complex body, and blank is bonded together mutually, and carries out infiltration reaction process to complex body.By multiple component are combined into parts can production size in a straightforward manner comparatively large and there are the complex-shaped parts such as hollow.
The invention provides a kind of relatively large and there is the production method compared with complicated shape ceramic component such as hollow with ceramic body reaction forming explained hereafter, especially the ceramic component production method based on RB-SiC, can obtain to compare with disclosed method by the method, in structure properties, there is higher homogeneity, and there is the ceramic component of less variable density and higher dimensional precision.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. the online reaction forming method of ceramic form, is characterized in that, comprise the following steps:
1) at least two ceramic forms be made up of carbonaceous material are respectively prepared;
2) prepare binding agent, described binding agent comprises the component of following weight percentage:
Water 25-35%, polyacrylamide 5-7%, tackiness agent 1-2%, silicon carbide micro-powder 30-45%, silica flour 10-20%, carbon dust 5-8%;
A, polyacrylamide to be added to the water, to stir and make it abundant dissolving, then add tackiness agent, configuration polyacrylamide solution;
B, silica flour, carbon dust and silicon carbide micro-powder to be added in polyacrylamide solution successively, be configured to slip;
C, then ball milling is carried out to slip, obtain binding agent;
3) at least two ceramic forms are connected into a complex body by least one joint face, coated with adhesive between the joint face of ceramic form, is then cured, dry after solidification, obtains composite body;
4) the composite body infiltration reaction after solidification is formed ceramic component.
2. the online reaction forming method of ceramic form according to claim 1, it is characterized in that, described infiltration reaction is included on the joint face between ceramic form and ceramic form and places silicon or silicon alloy, then by placing composite body siliconising process at the temperature of 1350 DEG C-1700 DEG C of silicon or silicon alloy, the bulk ceramics parts making the carbon in ceramic form and binding agent and silicon reaction in－situ generate silicon B-carbide to be combined.
3. the online reaction forming method of ceramic form according to claim 2, is characterized in that, the time of described siliconising process is 1-3 hour.
4. the online reaction forming method of ceramic form according to claim 1, it is characterized in that, described binding agent comprises the component of following weight percentage:
Water 35%, polyacrylamide 7%, tackiness agent 2%, silicon carbide micro-powder 30%, silica flour 20%, carbon dust 6%.
5. the online reaction forming method of ceramic form according to claim 1, it is characterized in that, described silicon carbide micro-powder comprises the silicon carbide micro-powder of the first granularity and the silicon carbide micro-powder of the second granularity, the granularity of the silicon carbide micro-powder of described first granularity is 1-10 μm, the granularity of the silicon carbide micro-powder of described second granularity is 20-40 μm, and the mass ratio of the silicon carbide micro-powder of described first granularity and the silicon carbide micro-powder of described second granularity is 1-2:1.
6. the online reaction forming method of the ceramic form according to any one of claim 1-5, it is characterized in that, described solidification is at room temperature carried out, and described drying comprises places the ceramic form after bonding in an oven, the temperature of described drying is 110-130 DEG C, and the dry time is 3-5 hour.
7. the online reaction forming method of ceramic form according to claim 6, is characterized in that, also comprise:
After coated with adhesive, joint face is pressurizeed between the joint face of ceramic form, or aim at when using frock to form connecting sewing to the ceramic body connected between joint face, then use binding agent to fill connecting sewing, finally the ceramic form connected is cured.
8. the online reaction forming method of ceramic form according to claim 7, is characterized in that, described step 1) comprising: utilize existing silicon carbide ceramics gel casting technology, the carbon containing ceramic blank needed for preparation;
Ceramic form is processed, utilizes numerical control machining center, adopt diamond cutter to process single silicon carbide ceramics blank;
Finally utilize binding agent, the above-mentioned ceramic form processed is connected into the composite body with hollow structure.
9. the online reaction forming method of ceramic form according to claim 8, is characterized in that, the time of described ball milling is 15-25 hour.
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| CN105585325B (en) * | 2015-12-24 | 2018-11-06 | 中国航空工业集团公司北京航空材料研究院 | A kind of silicon-carbon element original position reaction forming technique of carbon/silicon carbide ceramic matrix composite |
| CN108218462A (en) * | 2016-12-22 | 2018-06-29 | 中国科学院上海硅酸盐研究所 | Resin based sizing and SiC ceramic reaction forming method |
| CN108794041A (en) * | 2017-05-02 | 2018-11-13 | 中国科学院上海硅酸盐研究所 | A kind of reaction-sintered CfThe method that/SiC ceramic matrix composite material is connected with synchronous reaction |
| CN107915494B (en) * | 2017-11-24 | 2021-02-05 | 航天材料及工艺研究所 | High-thermal-conductivity high-strength carbon-based composite material and preparation method thereof |
| CN110304935B (en) * | 2019-08-08 | 2021-11-26 | 贵州大学 | Packaging method of ceramic microchannel |
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| CN101885618B (en) * | 2010-08-19 | 2013-03-06 | 哈尔滨工业大学 | Connection method of reactive sintered silicon carbide ceramics |
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