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CN107043263A - A kind of preparation method of low-temperature pressureless sintering silicon nitride ceramics - Google Patents

A kind of preparation method of low-temperature pressureless sintering silicon nitride ceramics Download PDF

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CN107043263A
CN107043263A CN201710283968.3A CN201710283968A CN107043263A CN 107043263 A CN107043263 A CN 107043263A CN 201710283968 A CN201710283968 A CN 201710283968A CN 107043263 A CN107043263 A CN 107043263A
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silicon nitride
sintering
temperature
low
preparation
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李晓雷
赵志浩
孙永强
季惠明
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Tianjin University
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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Abstract

The present invention relates to a kind of preparation method of low-temperature pressureless sintering silicon nitride ceramics；On the basis of alpha silicon nitride and sintering aid total amount, the mass content of alpha silicon nitride is 75 97%, and it is 3 25% to add sintering aid mass content, by mixed powder ball milling mixing, drying；By mixed powder by granulation, shaping, prepared sintered body is prepared；After preparation sintered body dumping, in 1,500 1600 DEG C of sintering, silicon nitride ceramic material is obtained.Low-temperature sintering silicon nitride ceramics prepared by the present invention, overcome the high shortcoming of traditional rare earth oxide sintering aid sintering temperature, relative density 98% can be obtained under low-temperature sintering, bending strength 671MPa, alpha silicon nitride is fully converted into the silicon nitride ceramic material of beta silicon nitride.

Description

A kind of preparation method of low-temperature pressureless sintering silicon nitride ceramics
Technical field
The invention belongs to inorganic non-metallic ceramics field of material preparation, it is specifically related to one kind under sintering temperature and low, Prepare high beta-silicon nitride content, high density, the method for the silicon nitride ceramics of high bending strength.
Background technology
Silicon nitride is as a kind of new ceramic material, and its hardness is high, corrosion-resistant, wear-resistant, and strong with good high temperature Degree.With other ceramic phase ratios, silicon nitride ceramics proportion is small, thermal coefficient of expansion is low, thermal-shock resistance is good, fracture toughness is high.And have There are the bar-shaped β-Si of high length-diameter ratio3N4Crystal grain can play a part of self toughening, can further improve the fracture toughness of material.It is A kind of preferable high-temperature structural material and high-speed cutting tool ceramics material
But it is due to that silicon nitride is covalent compound, nitrogen-atoms has very low self-diffusion coefficient, it is difficult to densified sintering product, nothing Pressure sintering must produce liquid phase, activated sintering process at high temperature using sintering aid.The species of the sintering aid of silicon nitride is various, Generally there are metal oxide, rare earth oxide, salt etc..In order to not influence the performance particularly high-temperature behavior of silicon nitride ceramics, The addition of sintering aid is appropriate, and the second high phase of refractoriness is separated out under high temperature, it is ensured that the high-temperature behavior of material, therefore often Sintering aid is rare earth oxide and MgO, Al2O3(Zoran Krstic,Vladimir D.Krstic,Silicon nitride:the engineering material of the future,J.Mater.Sci.47(2012)535-552)。 But according to existing achievement in research (Jian-Feng Yang, Tatsuki Ohji, Koichi Niihara, Influence of Yttria–Alumina Content on Sintering Behavior and Microstructure of Silicon Nitride Ceramics,J.Am.Ceram.Soc.,83(2000)2094–2096；Hirokazu Yamamoto,Katunori Akiyama,Yuichiro Murakami,Densification behaviors and high-temperature characteristics of Si3N4sintered bodies using Al2O3–Yb2O3additives, J.Eur.Ceram.Soc.26 (2006) 1059-1067), rare earth oxide and Al2O3, MgO sintering aid in pressureless sintering bar Under part, sintering temperature need to can be only achieved 90%, when sintering temperature reaches more than 1650 degree higher than the relative density of 1600 degree of ceramics, α-Si3N4β-Si can be just completely transformed into3N4, therefore to obtain high β-Si3N4The silicon nitride ceramics of content, its pressureless sintering temperature Degree is all higher than 1650 degree substantially, and general sintering temperature is 1700-1800 DEG C.As can be seen that being prepared under the conditions of traditional pressureless sintering Silicon nitride ceramics needs excessive temperature, requires high to agglomerating plant, energy consumption is big, the preparation cost of the material greatly improved, and Other sintering processings instrument that for example hot pressed sintering, discharge plasma sintering need is increasingly complex, costliness, and can not prepare complexity Shaped samples, processing loss is big, and cost is more expensive.And this research and utilization rare earth fluoride and Al2O3, MgO mixture be used as burning Auxiliary agent is tied, can be i.e. sinterable comparatively dense at 1500 degree or so, and α-Si can be made3N4It is completely transformed into β-Si3N4, and Obtain with high-melting-point Re4Si2N2O7、Re10(SiO4)6O3The rare earth silica such as (Re is rare earth ion) nitrogen is mutually the sample of intergranular phase Product, it is ensured that the heat resistance of sample.
The content of the invention
Low-temperature sintering beta-silicon nitride content is low and resistance to elevated temperatures is poor, mechanical property is low asks based on solving by the present invention Topic under sintering temperature and low, prepares high beta-silicon nitride content, high bending strength, the silicon nitride of high-fracture toughness there is provided one kind The method of ceramics.
Concrete technical scheme of the present invention is as follows：
A kind of preparation method of low-temperature pressureless sintering silicon nitride ceramics；On the basis of α-siliconnitride and sintering aid total amount, The mass content of α-siliconnitride is 75-97%, and it is 3-25% to add sintering aid mass content, by mixed powder ball milling mixing, Dry；By mixed powder by granulation, shaping, prepared sintered body is prepared；After preparation sintered body dumping, in 1500-1600 DEG C sintering, obtain silicon nitride ceramic material.
Yttrium fluoride, lanthanum fluoride, cerium fluoride, gadolinium fluoride, dysprosium fluoride, fluorine that the sintering aid composition is content 2-15wt% Change ytterbium one kind therein, and add one kind in 1-10wt% magnesia, aluminum oxide.
It is preferred that being sintered 0.5-6 hours at 1500-1600 DEG C.
Low-temperature sintering silicon nitride ceramics prepared by the present invention, overcomes traditional rare earth oxide sintering aid sintering temperature high Shortcoming, can obtain relative density 98% under low-temperature sintering, and bending strength 671MPa, α-siliconnitride is fully converted into β-nitridation The silicon nitride ceramic material of silicon.Wherein ceramic relative density calculates mode and is：Relative density=sample rate/solid density, The solid density of different formulations is determined to calculate after phase content and obtained by XRD.
The present invention has some following advantage compared with prior art：
1. the present invention obtains high density, high mechanics first based on rare earth fluoride sintering aid in lower temperature The silicon nitride ceramics of performance；
2. the present invention is on the premise of low-temperature sintering, crystal boundary phase composition is controlled, it is ensured that its high temperature tolerance energy；
3. sintering temperature of the present invention is less than 1600 DEG C, temperature and the requirement to agglomerating plant are reduced, nitrogen is greatly reduced The preparation cost of SiClx ceramics；
4. the low-temperature sintering silicon nitride ceramics relative density of the present invention is up to 98%, bending strength 671MPa, α-siliconnitride Beta-silicon nitride ratio is changed into up to 100% silicon nitride ceramic material.
Brief description of the drawings
Fig. 1 is the microscopic appearance figure of embodiment 3；
Fig. 2 is the X-ray diffractogram of embodiment 5；
Fig. 3 is the microscopic appearance figure of embodiment 5；
Fig. 4 is the microscopic appearance figure of embodiment 12；
Fig. 5 is the X-ray diffractogram of embodiment 17.
Embodiment
Embodiment 1：
By α-siliconnitride, yttrium fluoride, magnesia with mass ratio 88:2:10 dispensings, gained mixed powder adds alcohol and poly- Zirconium oxide balls planetary ball mill is used after vinyl alcohol 4 hours, the consumption of wherein polyvinyl alcohol is：Powder：Polyvinyl alcohol=100: 1.25.After gained slurry is dried, 40 mesh sieves are crossed, pelletizing is obtained.It is small in 600 degree of dumpings 1.5 after granulation powder is molded When, obtain pre-sintered body.Sintered body is positioned in atmosphere furnace, protective atmosphere, silicon nitride and boron nitride powder are done using nitrogen Bedding and padding are done, are sintered, sintering temperature is 1550 degree, sintering time 3 hours.Gained sample relative density 91%, intensity 431MPa, beta-silicon nitride conversion ratio 95%, intergranular is mutually Y4Si2N2O7。
Embodiment 2：
Specific steps be the same as Example 1, but α-siliconnitride, yttrium fluoride, magnesia mass ratio are 92:7:1, sintering temperature is 1500 degree, sintering time 0.5 hour.Gained sample relative density 90%, intensity 342MPa, beta-silicon nitride conversion ratio 95% is brilliant Between mutually be Y4Si2N2O7。
Embodiment 3：
Specific steps be the same as Example 1, but α-siliconnitride, yttrium fluoride, quality of alumina ratio are 80:15:5, sintering temperature is 1550 degree, sintering time 2 hours.Gained sample relative density 97%, intensity 492MPa, beta-silicon nitride conversion ratio 100%, intergranular It is mutually Y4Si2N2O7, the microscopic appearance figure of sample is as shown in Figure 1.
Embodiment 4：
Specific steps be the same as Example 1, but α-siliconnitride, lanthanum fluoride, magnesia mass ratio are 93:2:5, sintering temperature is 1600 degree, sintering time 6 hours.Gained sample relative density 97%, intensity 580MPa, beta-silicon nitride conversion ratio 95%, intergranular It is mutually La10(SiO4)6O3。
Embodiment 5：
Specific steps be the same as Example 1, but α-siliconnitride, lanthanum fluoride, quality of alumina ratio are 88:7:5, sintering temperature is 1500 degree, sintering time 6 hours.Gained sample relative density 90%, intensity 392MPa, beta-silicon nitride conversion ratio 68%, intergranular It is mutually La10(SiO4)6O3, as shown in Figure 2, microscopic appearance figure is as shown in Figure 3 for the X ray diffracting spectrum of sample.
Embodiment 6：
Specific steps be the same as Example 1, but α-siliconnitride, lanthanum fluoride, quality of alumina ratio are 84:15:1, sintering temperature is 1500 degree, sintering time 6 hours.Gained sample relative density 92%, intensity 424MPa, beta-silicon nitride conversion ratio 96%, intergranular It is mutually La10(SiO4)6O3。
Embodiment 7：
Specific steps be the same as Example 1, but α-siliconnitride, cerium fluoride, magnesia mass ratio are 97:2:1, sintering temperature is 1600 degree, sintering time 6 hours.Gained sample relative density 90%, intensity 467MPa, beta-silicon nitride conversion ratio 84%, intergranular It is mutually Ce4.667(SiO4)3O。
Embodiment 8：
Specific steps be the same as Example 1, but α-siliconnitride, cerium fluoride, magnesia mass ratio are 88:7:5, sintering temperature is 1550 degree, sintering time 3 hours.Gained sample relative density 95%, intensity 477MPa, beta-silicon nitride conversion ratio 82%, intergranular It is mutually Ce4.667(SiO4)3O。
Embodiment 9：
Specific steps be the same as Example 1, but α-siliconnitride, cerium fluoride, quality of alumina ratio are 75:15:10, sintering temperature is 1550 degree, sintering time 6 hours.Gained sample relative density 97%, intensity 580MPa, beta-silicon nitride conversion ratio 100%, intergranular It is mutually Ce4.667(SiO4)3O。
Embodiment 10：
Specific steps be the same as Example 1, but α-siliconnitride, gadolinium fluoride, quality of alumina ratio are 97:2:1, sintering temperature is 1500 degree, sintering time 6 hours.Gained sample relative density 88%, intensity 326MPa, beta-silicon nitride conversion ratio 70%, intergranular It is mutually GdSiNO2。
Embodiment 11：
Specific steps be the same as Example 1, but α-siliconnitride, gadolinium fluoride, magnesia mass ratio are 83:7:10, sintering temperature is 1600 degree, sintering time 6 hours.Gained sample relative density 95%, intensity 517MPa, beta-silicon nitride conversion ratio 100%, intergranular It is mutually GdSiNO2。
Embodiment 12：
Specific steps be the same as Example 1, but α-siliconnitride, gadolinium fluoride, magnesia mass ratio are 75:15:10, sintering temperature is 1600 be degree, sintering time 6 hours.Gained sample relative density 98%, intensity 671MPa, beta-silicon nitride conversion ratio 100% is brilliant Between mutually be GdSiNO2, the microscopic appearance figure of sample is as shown in Figure 4.
Embodiment 13：
Specific steps be the same as Example 1, but α-siliconnitride, dysprosium fluoride, quality of alumina ratio are 93:2:5, sintering temperature is 1600 degree, sintering time 3 hours.Gained sample relative density 95%, intensity 593MPa, beta-silicon nitride conversion ratio 100%, intergranular It is mutually Dy4Si2N2O7。
Embodiment 14：
Specific steps be the same as Example 1, but α-siliconnitride, dysprosium fluoride, quality of alumina ratio are 83:7:10, sintering temperature is 1600 degree, sintering time 0.5 hour.Gained sample relative density 94%, intensity 556MPa, beta-silicon nitride conversion ratio 100% is brilliant Between mutually be Dy4Si2N2O7。
Embodiment 15：
Specific steps be the same as Example 1, but α-siliconnitride, dysprosium fluoride, magnesia mass ratio are 80:15:5, sintering temperature is 1600 degree, sintering time 6 hours.Gained sample relative density 97%, intensity 664MPa, beta-silicon nitride conversion ratio 100%, intergranular It is mutually Dy4Si2N2O7。
Embodiment 16：
Specific steps be the same as Example 1, but α-siliconnitride, fluorination ytterbium, quality of alumina ratio are 88:2:10, sintering temperature is 1600 degree, sintering time 3 hours.Gained sample relative density 91%, intensity 475MPa, beta-silicon nitride conversion ratio 100%, intergranular It is mutually Yb4Si2N2O7。
Embodiment 17：
Specific steps be the same as Example 1, but α-siliconnitride, fluorination ytterbium, quality of alumina ratio are 92:7:1, sintering temperature is 1550 degree, sintering time 2 hours.Gained sample relative density 93%, intensity 476MPa, beta-silicon nitride conversion ratio 100%, intergranular It is mutually Yb4Si2N2O7, the X ray diffracting spectrum of sample is as shown in Figure 5.
Embodiment 18：
Specific steps be the same as Example 1, but α-siliconnitride, fluorination ytterbium, magnesia mass ratio are 84:15:1, sintering temperature is 1500 degree, sintering time 2 hours.Gained sample relative density 93%, intensity 483MPa, beta-silicon nitride conversion ratio 72%, intergranular It is mutually Yb4Si2N2O7。

Claims (3)

1. a kind of preparation method of low-temperature pressureless sintering silicon nitride ceramics；It is characterized in that using α-siliconnitride and sintering aid total amount as Benchmark, the mass content of α-siliconnitride is 75-97%, and it is 3-25% to add sintering aid mass content, by mixed powder ball milling Mix, dry；By mixed powder by granulation, shaping, prepared sintered body is prepared；After preparation sintered body dumping, in 1500- 1600 DEG C of sintering, obtain silicon nitride ceramic material.
2. the method as described in claim 1, it is characterized in that the yttrium fluoride that it is content 2-15wt% that sintering aid, which is constituted, fluorination Lanthanum, cerium fluoride, gadolinium fluoride, dysprosium fluoride, fluorination ytterbium one kind therein, and add in 1-10wt% magnesia, aluminum oxide one Kind.
3. the method as described in claim 1, it is characterized in that being sintered 0.5-6 hours at 1500-1600 DEG C.
CN201710283968.3A 2017-04-26 2017-04-26 A kind of preparation method of low-temperature pressureless sintering silicon nitride ceramics Pending CN107043263A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110240131A (en) * 2019-05-13 2019-09-17 天津炜润达新材料科技有限公司 A kind of preparation method of silicon nitride
CN113735563A (en) * 2021-08-10 2021-12-03 上海理工大学 Probe material for ultrasonic metallurgy and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101100388A (en) * 2007-07-17 2008-01-09 清华大学 High heat conductivity silicon nitride ceramics material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN101100388A (en) * 2007-07-17 2008-01-09 清华大学 High heat conductivity silicon nitride ceramics material and preparation method thereof

Non-Patent Citations (1)

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吴伟骏: "氮化硅陶瓷的制备及其耐腐蚀性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110240131A (en) * 2019-05-13 2019-09-17 天津炜润达新材料科技有限公司 A kind of preparation method of silicon nitride
CN113735563A (en) * 2021-08-10 2021-12-03 上海理工大学 Probe material for ultrasonic metallurgy and preparation method thereof
CN113735563B (en) * 2021-08-10 2022-10-18 上海理工大学 Probe material for ultrasonic metallurgy and preparation method thereof

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Application publication date: 20170815