CN104030686B - A kind of high tenacity silicon carbide ceramics and preparation method thereof - Google Patents
A kind of high tenacity silicon carbide ceramics and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of high tenacity silicon carbide ceramics and preparation method thereof, this high tenacity silicon carbide ceramics by the toughner titanium carbide of 3-5%, the sintering aid of 1-4% and surplus silicon carbide and inevitably impurity form, wherein sintering aid is 1:(0.6-8 by mass percent) carbon and norbide form.Its preparation method is first by silicon carbide, toughner titanium carbide, sintering aid carbon and norbide mix puts into ball mill, add water soluble resin and distilled water carries out ball milling, then compression moulding in punching block is joined after drying, put in vacuum oven after shaping and sinter, obtained the finished product high tenacity silicon carbide ceramics after finally carrying out surface grinding processing.The present invention adds toughner titanium carbide in silicon carbide substrate, making the fracture mode of thyrite be main transformer from grain boundary fracture is based on transgranular fracture, improve the energy needed for transcrystalline and grain boundary fracture, thus serve the effect strengthening folding strength.
Description
Technical field
The present invention relates to a kind of pottery and preparation method thereof, particularly relate to a kind of high tenacity silicon carbide ceramics and preparation method thereof.
Background technology
Along with the development of science and technology, the requirements of field to material such as sealing, armoring industry are more and more harsher, in the urgent need to developing a kind of novel high performance material.And silicon carbide ceramics has very high intensity and creep resistance at normal temperatures, excellent oxidation-resistance and erosion resistance, and also silicon carbide ceramics has extremely low frictional coefficient, and wear resistance is very excellent, has wide market outlook.
But silicon carbide ceramics fragility is comparatively large, and fracture toughness property is lower, normal pressure-sintered silicon carbide ceramics folding strength, generally at about 400MPa, is difficult to meet the field such as sealing, armoring industry to the demand of the silicon carbide ceramics of high tenacity, high strength.
Summary of the invention
The object of the invention is for the above-mentioned problems in the prior art, propose the silicon carbide ceramics of a kind of high tenacity, high breaking strength.
Object of the present invention realizes by following technical proposal: a kind of high tenacity silicon carbide ceramics, described high tenacity silicon carbide ceramics is become to be grouped into by following mass percent: toughner: 3-5%, sintering aid: 1-4%, surplus is silicon carbide and inevitable impurity.
Because silicon carbide ceramics fragility is comparatively large, fracture toughness property is lower, and normal pressure-sintered silicon carbide ceramics folding strength only has about 400MPa, and being not enough to meet has the field of more high strength demand to use to silicon carbide ceramics.Therefore, the present invention adds the toughner of 3-5% in silicon carbide, carries out modification to the toughness of silicon carbide, thus improves the folding strength of silicon carbide.But, again because silicon carbide is strong covalent bond compound, and at high temperature still can keep very high bond strength, its self-diffusion coefficient is very little, the necessary volume diffusion of densification and grain boundary decision speed very little, simultaneously crystal boundary energy and powder surface can odds ratio ionic compound and metal much bigger, make to sinter motivating force less.Therefore, the present invention adds a small amount of sintering aid, in high-temperature sintering process, improve surface energy, impels product to sinter DB into.
As preferably, described toughner is titanium carbide.The fracture of silicon carbide ceramics matrix material is mostly grain boundary fracture, and after adding toughner titanium carbide, titanium carbide is evenly distributed in silicon carbide ceramics matrix crystal grain, and part is positioned at grain boundaries, forms " intracrystalline shape " and " intergranular shape " mixed distribution.Because partially carbonized titanium is positioned at crystal grain, in crystal grain, produce tension stress, be easy to produce subgrain boundary, its fracture mode is mostly transgranular fracture.As can be seen here, titanium carbide is added in silicon carbide ceramics matrix, by the disperse of titanium carbide granule, form " intracrystalline shape " and " intergranular shape " and mix shape distribution, making the fracture mode of thyrite be main transformer from grain boundary fracture is based on transgranular fracture, enhance the intensity of crystal boundary, improve the energy needed for transcrystalline and grain boundary fracture, thus serve the effect strengthening folding strength.In addition, when crackle is expanded in silicon carbide ceramics matrix, the unrelieved stress that particle produces can change the route of transmission of crackle, makes crack deflection.
As preferably, described sintering aid comprises carbon and norbide, and the mass percent of described carbon, norbide is 1:(0.6-8).Because the high covalency key in silicon carbide and low diffustivity make it be difficult to sintering when not having sintering aid.So the present invention adds the sintering aid mixed by carbon and norbide on a small quantity, improves powder surface and can impel densified sintering product in high-temperature sintering process.
As preferably, described silicon carbide particle diameter is 0.3-2 μm, and described toughner titanium carbide particle diameter is 1-3 μm, and the particle diameter of described sintering aid carbon and norbide is 1-5 μm.The silicon carbide that the present invention chooses, toughner and sintering aid particle diameter are all micron-sized, therefore, can ensure the grain fineness number after silicon carbide ceramics sintering, be conducive to the volume density and the mechanical strength that improve silicon carbide ceramics.
Another object of the present invention is the preparation method providing above-mentioned high tenacity silicon carbide ceramics, and described preparation method comprises the following steps:
S1, take silicon carbide by mass percentage, toughner titanium carbide, sintering aid carbon and norbide also mix;
S2, the above-mentioned powder mixed is put into ball mill, add the water soluble resin of 1-6%, the distilled water of 80%-140% carries out ball milling;
S3, with steam drying cabinet by powder good for above-mentioned ball milling dry, after oven dry, powder is joined in punching block, is pressurized to 150-250MPa/cm
2compression moulding, the press time is 1-10s;
S4, to be put in vacuum oven by the biscuit after above-mentioned compression moulding and sinter, sintering temperature is 2100-2200 DEG C, and soaking time is 1-3 hour;
S5, the biscuit after above-mentioned sintering carried out surface grinding processing after obtained the finished product high tenacity silicon carbide ceramics.
As preferably, in step S2, the ratio of grinding media to material of ball milling is 3:1, and Ball-milling Time is 2h.
As preferably, in step S3, pressing pressure is 150-200MPa/cm
2, the press time is 2-5s.
As preferably, in step S4, sintering temperature is 2150 DEG C, and soaking time is 1-2 hour.
The preparation method of high tenacity silicon carbide ceramics of the present invention is simple, and the present invention strictly controls the Parameter Conditions in the processes such as ball milling, compression moulding and sintering, ensure the good mechanical performance such as the intensity of final obtained silicon carbide ceramics product, creep resistance, oxidation-resistance, abrasion resistance and erosion resistance.
The present invention has the following advantages:
1. high tenacity silicon carbide ceramics of the present invention is in silicon carbide substrate, add the toughner titanium carbide of 3-5%, by the disperse of titanium carbide granule, form " intracrystalline shape " and " intergranular shape " and mix shape distribution, making the fracture mode of thyrite be main transformer from grain boundary fracture is based on transgranular fracture, enhance the intensity of crystal boundary, improve the energy needed for transcrystalline and grain boundary fracture, thus serve the effect strengthening folding strength.
2. high tenacity silicon carbide ceramics of the present invention also adds the sintering aid be made up of certain proportion carbon and norbide in the base, improves powder surface and can impel and sinter DB in high-temperature sintering process.
3. high tenacity silicon carbide ceramics raw material particle size of the present invention is little, can ensure the grain fineness number of silicon carbide ceramics after sintering, is conducive to the volume density and the mechanical strength that improve silicon carbide ceramics.
4. the preparation method of high tenacity silicon carbide ceramics of the present invention is simple, by strictly controlling the conditional parameter in preparation process, make that final obtained silicon carbide ceramics product strength is large, creep resistance, oxidation-resistance, the good mechanical performance such as abrasion resistance and erosion resistance.
Embodiment
Be below specific embodiments of the invention, technical scheme of the present invention is further described, but the present invention is not limited to these embodiments.
Table 1: embodiment of the present invention 1-4 high tenacity silicon carbide ceramics
Moiety and mass percent thereof
Embodiment 1:
Taking particle diameter by the moiety of embodiment in table 11 high tenacity silicon carbide and mass percent thereof is the silicon carbide of 0.3-0.6 μm, the titanium carbide of 1-1.5 μm, and the sintering aid carbon of 1-2 μm and norbide also mix.Put into ball mill after mixing, controlling ratio of grinding media to material is 3:1, and adds the water soluble resin of 3%, and the distilled water of 80% carries out ball milling 2h.Ball milling terminates rear steam drying cabinet dries powder, then joins in punching block, is pressurized to 150MPa/cm
2compression moulding, the press time controls as 4s.Then put in vacuum oven by the biscuit after compression moulding and sinter, it is 2130 DEG C that sintering temperature controls, and soaking time is 3 hours.The finished product high tenacity silicon carbide ceramics is obtained after finally the biscuit after sintering being carried out surface grinding processing.
Embodiment 2:
Taking particle diameter by the moiety of embodiment in table 12 high tenacity silicon carbide and mass percent thereof is the silicon carbide of 0.6-1.0 μm, the titanium carbide of 1.3-1.6 μm, and the sintering aid carbon of 1.5-2.5 μm and norbide also mix.Put into ball mill after mixing, controlling ratio of grinding media to material is 3:1, and adds the water soluble resin of 4%, and the distilled water of 100% carries out ball milling 2h.Ball milling terminates rear steam drying cabinet dries powder, then joins in punching block, is pressurized to 180MPa/cm
2compression moulding, the press time controls as 2s.Then put in vacuum oven by the biscuit after compression moulding and sinter, it is 2150 DEG C that sintering temperature controls, and soaking time is 2 hours.The finished product high tenacity silicon carbide ceramics is obtained after finally the biscuit after sintering being carried out surface grinding processing.
Embodiment 3:
Taking particle diameter by the moiety of embodiment in table 13 high tenacity silicon carbide and mass percent thereof is the silicon carbide of 0.8-1.3 μm, the titanium carbide of 1.5-2 μm, and the sintering aid carbon of 2-2.5 μm and norbide also mix.Put into ball mill after mixing, controlling ratio of grinding media to material is 3:1, and adds the water soluble resin of 5%, and the distilled water of 120% carries out ball milling 2h.Ball milling terminates rear steam drying cabinet dries powder, then joins in punching block, is pressurized to 160MPa/cm
2compression moulding, the press time controls as 3s.Then put in vacuum oven by the biscuit after compression moulding and sinter, it is 2160 DEG C that sintering temperature controls, and soaking time is 2 hours.The finished product high tenacity silicon carbide ceramics is obtained after finally the biscuit after sintering being carried out surface grinding processing.
Embodiment 4:
Taking particle diameter by the moiety of embodiment in table 14 high tenacity silicon carbide and mass percent thereof is the silicon carbide of 1.0-1.6 μm, the titanium carbide of 2.0-2.5 μm, and the sintering aid carbon of 3-4 μm and norbide also mix.Put into ball mill after mixing, controlling ratio of grinding media to material is 3:1, and the distilled water adding the water soluble resin 140% of 6% carries out ball milling 2h.Ball milling terminates rear steam drying cabinet dries powder, then joins in punching block, is pressurized to 150MPa/cm
2compression moulding, the press time controls as 6s.Then put in vacuum oven by the biscuit after compression moulding and sinter, it is 2180 DEG C that sintering temperature controls, and soaking time is 1 hour.The finished product high tenacity silicon carbide ceramics is obtained after finally the biscuit after sintering being carried out surface grinding processing.
The high tenacity silicon carbide ceramics of the present invention that above-described embodiment 1-4 is obtained carries out performance test, and test result is as shown in table 2.
As can be seen from Table 2, the high tenacity silicon carbide ceramics volume density that obtains of the present invention is at 3.1-3.3g/cm
3between, compactness is high, and after adding toughner titanium carbide, the folding strength of silicon carbide ceramics brings up to more than 480MPa from about 400MPa, intensity improves clearly, and the Shore hardness of silicon carbide ceramics, compressive strength, Young's modulus and thermal expansivity all make moderate progress, thus the corrosion-resistant, wear-resisting of silicon carbide ceramics and thermostability are increased.Therefore, the performance boost of high tenacity silicon carbide ceramics of the present invention is very large, be enough to meet the field such as sealing, armoring industry to the demand of the silicon carbide ceramics of high tenacity, high strength, fill up the vacancy of high tenacity on market, high-strength carborundum ceramic product, development prospect is boundless.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Although made a detailed description the present invention and quoted some specific embodiments as proof, to those skilled in the art, only otherwise it is obvious for leaving that the spirit and scope of the present invention can make various changes or revise.
Claims (5)
1. a high tenacity silicon carbide ceramics, is characterized in that, described high tenacity silicon carbide ceramics is become to be grouped into by following mass percent: toughner: 3-5%, sintering aid: 1-4%, and surplus is silicon carbide and inevitable impurity; Wherein, described sintering aid comprises carbon and norbide, and the mass percent of described carbon, norbide is arbitrary in 3:0.4,3:0.6,2.5:1.0 or 3.0:0.8, and particle diameter is 1-5 μm; Described toughner is titanium carbide, and particle diameter is 1-3 μm; Described silicon carbide particle diameter is 0.3-2 μm.
2. a preparation method for high tenacity silicon carbide ceramics as claimed in claim 1, is characterized in that, described preparation method comprises the following steps:
S1, take silicon carbide by mass percentage, toughner titanium carbide, sintering aid carbon and norbide also mix;
S2, the above-mentioned powder mixed is put into ball mill, add the water soluble resin of 1-6%, the distilled water of 80%-140% carries out ball milling;
S3, with steam drying cabinet by powder good for above-mentioned ball milling dry, after oven dry, powder is joined in punching block, is pressurized to 150-250MPa/cm
2compression moulding, the press time is 1-10s;
S4, to be put in vacuum oven by the biscuit after above-mentioned compression moulding and sinter, sintering temperature is 2100-2200 DEG C, and soaking time is 1-3 hour;
S5, the biscuit after above-mentioned sintering carried out surface grinding processing after obtained the finished product high tenacity silicon carbide ceramics.
3. the preparation method of a kind of high tenacity silicon carbide ceramics according to claim 2, is characterized in that, in step S2, the ratio of grinding media to material of ball milling is 3:1, and Ball-milling Time is 2h.
4. the preparation method of a kind of high tenacity silicon carbide ceramics according to claim 2, is characterized in that, in step S3, pressing pressure is 150-200MPa/cm
2, the press time is 2-5s.
5. the preparation method of a kind of high tenacity silicon carbide ceramics according to claim 2, is characterized in that, in step S4, sintering temperature is 2150 DEG C, and soaking time is 1-2 hour.
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CN105669205B (en) * | 2014-11-17 | 2018-04-13 | 中国科学院上海硅酸盐研究所 | The method that fine and close solid-phase sintered silicon carbide is prepared using grain composition powder as raw material |
CN104989827A (en) * | 2015-06-17 | 2015-10-21 | 宁波东联密封件有限公司 | Mechanical sealing device for pump |
CN105948754B (en) * | 2016-05-03 | 2019-02-22 | 浙江东新新材料科技有限公司 | The method that reaction-sintered prepares fine grain silicon carbide ceramics |
CN107573076B (en) * | 2017-09-18 | 2020-05-22 | 山东理工大学 | High-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped piece |
CN107619282B (en) * | 2017-09-18 | 2020-06-09 | 山东理工大学 | Preparation method of high-toughness titanium silicon carbide-silicon carbide complex phase ceramic special-shaped part |
CN114478014A (en) * | 2020-10-26 | 2022-05-13 | 深圳市万普拉斯科技有限公司 | Silicon carbide ceramic material, ceramic mold and preparation method thereof |
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CN101555143A (en) * | 2009-05-12 | 2009-10-14 | 宁波欧翔精细陶瓷技术有限公司 | Preparation method of normal pressure-sintered silicon carbide ceramics |
CN102390999A (en) * | 2011-08-10 | 2012-03-28 | 武汉钢铁(集团)公司 | Liquid-phase-sintered SiC-TiC composite ceramic and preparation method thereof |
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CN102390999A (en) * | 2011-08-10 | 2012-03-28 | 武汉钢铁(集团)公司 | Liquid-phase-sintered SiC-TiC composite ceramic and preparation method thereof |
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