CN101244936B - Injection mold SiC ceramic preliminary shaping blank method for reinforcing metallic infiltration - Google Patents
Injection mold SiC ceramic preliminary shaping blank method for reinforcing metallic infiltration Download PDFInfo
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- CN101244936B CN101244936B CN2008101025231A CN200810102523A CN101244936B CN 101244936 B CN101244936 B CN 101244936B CN 2008101025231 A CN2008101025231 A CN 2008101025231A CN 200810102523 A CN200810102523 A CN 200810102523A CN 101244936 B CN101244936 B CN 101244936B
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Abstract
The invention belongs to the research field of metal matrix composite, providing a strengthening method for the injected shaped SiC ceramic preliminary bland through the infiltration of metal like Cu or Al, which is characterized by putting the SiC injected blank formed through the injection of a wax-based binder system into natrium water glass solution with the concentration of 0.8 percent to 1.2 percent by weight and the modulus of 2.2 to 2.5 after solvent degreasing and partial thermal degreasing, uniformly impregnating and taking out to dry at the room temperature, and going on with the thermal degreasing until the left binder in the blank being eliminated completely before impregnation, and the degreasing process is divided into two processes, first, thermal degreasing, the temperature is controlled between 350 to 380 DEG C, the degreasing time is 0.5 to 2 hours, then impregnating and drying process is carried on, in the second degreasing process, the temperature is controlled between 550 to 600 DEG C, the degreasing time is 0.5 to 2 hours, in the process, the blank is increased to 4 MPa from the 0.2MPa which is carried out before the strengthening process so as to satisfy operating requirements better, the method can not only strengthen the intensity of the blank effectively but also has comparatively less foreign substances, which has no obvious influence on the properties of the finally produced composite materials.
Description
Technical field
The invention belongs to field of research of metal, relate to the method for a kind of reinforcing metallic infiltration with injection mold SiC ceramic preliminary shaping blank.
Background technology
High-volume fractional SiCp/Al or SiCp/Cu matrix material have excellent heat physical properties such as high heat conductance, low thermal coefficient of expansion and high ratio modulus, are a kind of very ideal electronic package materials.But characteristics such as the high rigidity that this kind material itself has, high fragility make its device that is difficult to be processed into by the method for secondary machine required shape, have limited being extensive use of of this kind material so greatly.Therefore the near-net-shape technology of developing this kind material is very necessary.At present both at home and abroad institute extensively the near-net-shape technology of employing be the liquid metal method of impregnation, be exactly to prepare porous wild phase ceramic body earlier with net shape, by infiltration process the Al of molten state or Cu metal and porous ceramics base are combined then, form final matrix material.From the characteristics of this technology, realize that can the near-net-shape of matrix material depend on the near-net-shape that realize the wild phase ceramic body.And adopt the ceramic powder injection molding process can realize the near-net-shape of SiC ceramic body well, and prepared base substrate dimensional precision height, production cost is low.
In the ceramic powder injection molding process, wax-based binder is a kind of binder system of extensive employing, and this binding agent has good temperature flowing and room temperature conformality, and can remove clean in 550 ℃～600 ℃ scopes.And infiltration normally carries out in 1000 ℃～1400 ℃ temperature ranges, in order to guarantee the efficient of each step process, degreasing is normally carried out in different atmosphere and stove with infiltration, so just need carry the degreasing base, operation such as shove charge, and injection forming SiC degreasing base is not owing to add any sintering aid (add sintering aid and can influence final prepared performance of composites), and temperature is lower, this moment, the intensity of base substrate was also very low, be difficult to get operations such as stove, shove charge, therefore must carry out intensified operation base substrate.Both at home and abroad at present extensively the method that adopts is to adopt the method for SiC base substrate high temperature oxidation, promptly calcine the SiC base substrate by at high temperature (＞900 ℃) in air, at SiC particle surface formation one deck non-crystalline state SiO
2Layer, the SiO that produces between the SiC particle
2The mutual bonding of layer is the main source of blank strength.But there is certain deficiency in this method, is exactly Al alloy-based cognition and SiO in the process of infiltration
2Layer reacts, and generates the MgAl of heat conductivility difference at the interface at SiC/Al
2O
4Phase has hindered the transmission of heat at the interface, thereby has influenced the heat conductivility of final matrix material.
Summary of the invention
Inorganic adhesive is as a kind of reinforcing aids that adds, as silicates, phosphoric acid salt, colloid silica etc., ceramic and as the binding agent of refractory materials and sand mold casting has been widely used at present boning, be characterized in bonding strength height, good operation performance, solidification value can be that room temperature also can be the middle low temperature below 300 ℃.Based on this, the present invention adopt a kind of in sand mold casting, extensively adopt tackiness agent---water glass is as the reinforcing aids of injection forming SiC degreasing base, by adopting the dehydration of water glass dipping base substrate after drying, can strengthen the SiC base substrate effectively, blank strength is increased to 4MPa by the 0.2MPa before not strengthening, and can satisfy operational requirement preferably.This kind method not only can increase blank strength effectively, and the impurity of introducing is less, can not produce tangible influence to final prepared performance of composites.
Concrete technology is:
At first, SiC powder and an amount of polymer wax-based binder are mixed on mixing roll, granulate then, in certain temperature and pressure scope, inject, obtain the injection base of desired shape; Base substrate be will inject afterwards and solvent degreasing, hot degreasing process carried out.For the ease of carrying out dip operation, the degreasing base should possess certain intensity, but also should possess certain porosity simultaneously, to guarantee that solution can be impregnated in the base substrate.Therefore, degreasing process is divided into two the step carry out: at first carry out the portion of hot degreasing, slowly be warming up to 350 ℃～380 ℃, degreasing time is 0.5～2 hour, to remove most paraffin and high density polyethylene(HDPE); To put in the sodium silicate solution that concentration is 0.8wt%～1.2wt%, modulus 2.2～2.5 through the base substrate of portion of hot degreasing then, after dipping under the room temperature is even, take out dry; Proceed hot degreasing afterwards, skimming temp is controlled at 550 ℃～600 ℃, and remaining binding agent removes fully in the base substrate before dipping, and degreasing time is 0.5～2 hour.Though do not have binding agent in the base substrate this moment, owing to added water glass in the process of degreasing, base substrate can well be strengthened.
The invention has the advantages that operation just can be strengthened degreasing blank preferably under lower temperature, and it is less to introduce impurity level, and performance of composites is not produced tangible influence.As when preparing the 67vol%SiCp/Al matrix material, employing concentration is that the water glass dipping SiC volume fraction of 0.8wt% is the degreasing blank of 67vol%, blank strength can reach 3.9MPa after drying, and the base substrate weightening finish has only 0.45wt%, and the amount of just introducing impurity is 0.45wt%; Thermal conductivity through the prepared SiCp/Al matrix material of later stage infiltration can reach 190W/ (mK), and (194W/ (mK)) is similar for the thermal conductivity of the SiCp/Al matrix material corresponding with the original base substrate that does not adopt any Enhancement Method.And adopt oxidation style to strengthen base substrate, and when reaching the intensity of 3.9MPa equally, need be 1100 ℃ of oxidations 3 hours, the weightening finish of base substrate is about 0.9wt%, and the thermal conductivity of prepared SiCp/Al matrix material has only 120W/ (mK).Therefore adopting water glass dipping SiC degreasing blank is a kind of cost-effective enhancement method.
Description of drawings:
Fig. 1 is a process flow sheet of the present invention.
Embodiment:
Embodiment 1: preparation intensity is that 4MPa, SiC volume fraction are the preform of 67vol%
The employing granularity is that the SiC powder of 60 μ m mixes with wax-based binder, the volume fraction of SiC is 67vol%, the main component of wax-based binder is 65wt%PW (paraffin)+30wt%HDPE (high density polyethylene(HDPE))+5wt%SA (stearic acid), obtain granulating after the uniform feeding part of the required shape that on injection moulding machine, is shaped afterwards.After will injecting base and carrying out solvent degreasing, be warmed up to 360 ℃ with the temperature rise rate of 5 ℃/min, also have part high density polyethylene(HDPE) not remove in the base substrate this moment, in order to keep blank strength.With this understanding, blank strength still reaches 5MPa, can satisfy the requirement of operations such as dipping and dehydration sclerosis to intensity.
To put into concentration through the base substrate of 360 ℃ of hot degreasings is that 0.8wt%, modulus are in 2.3 the sodium silicate, dipping evenly takes out dry in the back under room temperature, to put back to through dipping and exsiccant base substrate afterwards and proceed hot degreasing to 550 ℃ in the stove, to remove remaining binding agent such as remaining high density polyethylene(HDPE).With this understanding, the intensity of base substrate can reach 4MPa, and the foreign matter content in the base substrate only is 0.45wt%.
Embodiment 2: preparation intensity is that 9MPa, SiC volume fraction are the preform of 67vol%
The employing granularity is that the SiC powder of 60 μ m mixes with wax-based binder, the volume fraction of SiC is 67vol%, the main component of wax-based binder is 65wt%PW (paraffin)+30wt%PP (polypropylene)+5wt%SA (stearic acid), obtain granulating after the uniform feeding part of the required shape that on injection moulding machine, is shaped then.After will injecting base and carrying out solvent degreasing, be warmed up to 380 ℃ with the temperature rise rate of 5 ℃/min, also have polypropylene segment not remove in the base substrate this moment, in order to keep blank strength.With this understanding, blank strength can satisfy the requirement of operations such as dipping and dehydration sclerosis to intensity near 5MPa.
To put into concentration through the base substrate of 380 ℃ of hot degreasings is that 1.2wt%, modulus are in 2.3 the sodium silicate, dipping evenly takes out dry in the back under room temperature, to put back to through dipping and exsiccant base substrate afterwards and proceed hot degreasing to 550 ℃ in the stove, to remove remaining binding agent such as remaining polypropylene.With this understanding, the intensity of base substrate can reach 9MPa, and the foreign matter content in the base substrate only is 0.7wt%.
Claims (2)
1. a reinforcing metallic infiltration is with the method for SiC pottery preformation base substrate, it is characterized in that: after will adopting the SiC injection base process solvent degreasing and portion of hot degreasing of wax-based binder system injection forming, putting into concentration is the sodium silicate solution of 0.8wt%～1.2wt%, modulus 2.2～2.5, and dipping evenly takes out dry in the back under room temperature; Proceed afterwards hot degreasing before dipping in the base substrate remaining binding agent remove fully.
2. according to the method for the described a kind of reinforcing metallic infiltration of claim 1 with SiC pottery preformation base substrate, it is characterized in that: injection forming adopts wax-based binder, and hot degreasing was divided into for two steps, the hot degreasing of the first step, and temperature is controlled at 350 ℃～380 ℃; Degreasing time is 0.5～2 hour; Then the dipping, drying; Carry out the second hot degreasing of step afterwards, skimming temp is controlled at 550 ℃～600 ℃, and degreasing time is 0.5～2 hour.
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| CN2008101025231A CN101244936B (en) | 2008-03-24 | 2008-03-24 | Injection mold SiC ceramic preliminary shaping blank method for reinforcing metallic infiltration |
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| DE102013106276A1 (en) * | 2013-06-17 | 2014-12-18 | Ask Chemicals Gmbh | Lithium-containing molding material mixtures based on an inorganic binder for the production of molds and cores for metal casting |
| CN104451237A (en) * | 2014-11-14 | 2015-03-25 | 北京科技大学 | Method for preparing three-dimensional continuous network Cr3C2-Cu composites by utilizing infiltration process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016591A (en) * | 2007-03-08 | 2007-08-15 | 北京科技大学 | Method of preparing SiCp/Al composite material with complicated shape and high volume percent ratio |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101016591A (en) * | 2007-03-08 | 2007-08-15 | 北京科技大学 | Method of preparing SiCp/Al composite material with complicated shape and high volume percent ratio |
Non-Patent Citations (2)
| Title |
|---|
| 任淑彬,何新波,曲选辉.无压熔渗制备SiCp/Al复合材料的界面改性研究进展.材料科学与工艺13 5.2005,13(5),556-560. |
| 任淑彬,何新波,曲选辉.无压熔渗制备SiCp/Al复合材料的界面改性研究进展.材料科学与工艺13 5.2005,13(5),556-560. * |
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