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1、利用高炉水淬渣制备(Ca/Y)-Sialon 陶瓷的组织与性能论文作者 XX（XX大学 材料各向异性与织构教育部重点实验室，辽宁沈阳 XXXXXX）摘要：研究了以高炉水淬渣合成的Ca-Sialon粉体为原料制备(Ca/Y)-Sialon的烧结致密化过程、材料的力学性能、显微组织、相组成和材料的断裂特征。结果表明，适量的Y2O3 促进材料的烧结致密化和提高材料的力学性能，但 Y2O3（大于 10%）过量时对材料的烧结和力学性能不利。掺杂Y3+的(Ca/Y)-Sialon呈柱状晶，随着Y2O3含量的增加和烧结温度的提高，(Ca/Y)-Sialon呈柱状晶出现粗化和等轴化。含10Y2O3的材料在 1
2、700烧结时可获得较高的力学性能。关键词：(Ca/Y)-Sialon，水淬渣，无压烧结，力学性能，显微组织中图分类号:TQ174 高炉水淬渣是炼铁过程中产生的副产品，它的主要成分为SiO2、Al2O3、CaO和一些含 Fe杂质相，目前主要用于制造水泥。如何提高炉水淬渣的附加值，是人们梦寐以求的事情 1。目前利用高炉渣合成Sialon粉体已经进行了广泛的研究，如刘克明 2 等研究了利用高炉渣合成Ca-Sialon的热力学分析与工艺优化，姜涛等 3 研究了高炉渣合成Ca-Mg-Sialon的工艺参数，蒋久信等 4研究了炉渣 Ca-Sialon粉体的高温自蔓延燃烧合成工艺。但目前利用炉渣合成 Sia
3、lon 粉体无压烧结制备Sialon 陶瓷的性能还不高，并且工艺复杂，如陈卫武等 5 利用采用埋粉的方式无压烧结（1800）和热压烧结制备了（Ca，Mg）-Sialon陶瓷。Sialon 陶瓷具有优良的性能，在结构陶瓷方面具有广泛的用途，被认为是最有希望的结构陶瓷之一6。但由于-Sialon材料的高含氮量,名师资料总结-精品资料欢迎下载-名师精心整理-第 1 页，共 8 页 -给材料的无压烧结致密化带来一定的困难7.作为添加剂的金属离子在烧结后能进入-Sialon结构从而减少晶界相的含量,并改善材料的力学性能.最近的研究表明Y2O3可以降低陶瓷的烧结温度8.本工作以矿渣合成Ca-Sialon为
4、原料、以 Al2O3和 Y2O3为添加剂，研究了无压烧结(Ca/Y)-Sialon陶瓷的致密化行为、力学性能、相组成及显微结构，为矿渣的利用提供了新的途径。1 实验过程实验采用由高炉水淬渣合成的Ca-Sialon粉(上海宝田公司提供，主相为 Ca-Sialon,杂质主要为 Fe4N，同时还有 Cr、Mo、Mn等元素)为原料，以 Al2O3(平均粒径小于1m),Y2O3(含量为 99.9 wt%，平均粒径小于1m)为烧结助剂。试样中 Al2O3的含量为 5，Y2O3 的含量分别为4、6、8、10、12 和 14wt，成形粘结剂为聚乙烯醇，加入量为总质量的10。将按组份配置的初始粉料球磨混合 12
5、h，磨球为氧化铝球，介质为无水乙醇。球磨后的物料经干燥、造粒后，在 40MPa压力下单向预压成形（条样尺寸为6636mm），再在 200MPa 下冷等静压成形。成形坯体经10012h烘干后，在纯 0.1MPa的 N2气氛下烧结，烧结制度分别采用17001.5h 和 17501.5h 两种制度。利用阿基米德定律测定试样的体积密度。用理学D/max-rB 型 X射线衍射(X-ray diffraction，XRD)仪进行相组成分析。采用WD210 型电子万能试验机测量材料的三点弯曲强度,加载速率为 0.5mm/min。弯曲强度值取5 个样品的平均值。使用维氏硬度计测量材料的维氏硬度，加压载荷为 5
6、kg，取 4个样品的平均值。利用 SSX-550型扫描电镜观察试样的显微形貌，并利用EDX进行微区成分分析。采用 GX71金相显微镜进行组织分析。利用LEXT OLS3000激光扫描共聚焦显微镜进行材料断裂行为分析。2 结果与讨论名师资料总结-精品资料欢迎下载-名师精心整理-第 2 页，共 8 页 -2.1 不同 Y2O3 含量材料的烧结行为图 1 为试样的体积密度随Y2O3含量的变化曲线。由图可知，随着Y2O3含量的增加，试样的体积密度呈现先增加后降低的变化规律，不同Y2O3含量试样在1750烧结的密度均比1700烧结的低，当Y2O3含量含量为10、烧结温度为 1700时材料的体积密度最高为
7、3.32g/cm3。这是由于 Y2O3一方面其 Y3+和O2 容易固溶到Sialon 晶格中使 Sialon 晶格发生畸变 9，另一方面Y2O3与试样中添加的 Al2O3形成 YAG10，从而促进了材料的烧结行为.但当 Y2O3含量超过 10时，固熔于Sialon 中的量明显增加，使Sialon 的熔点大大降低，试样中易出现挥发物和气泡，使试样的密度降低，当烧结温度增加时，这种出现挥发物和气泡的情况也增加，因此试样的密度也降低。2.2 材料的力学性能图 2 和图 3 分别为 Y2O3含量对材料维氏硬度和抗折强度的影响曲线。由图可知，材料的维氏硬度和抗折硬度均随Y2O3含量的增加呈现先增加后降低
8、的变化趋势，这与 Y2O3含量对材料体积密度的影响规律（图1）相同，说明适量的Y2O3促进材料烧结，使材料的力学性能均提高，但Y2O3 含量过高使材料密度降低，因此材料的力学性能也降低。从图2 和图 3 还可以看出，烧结温度对维氏硬度的影响与 Y2O3含量有关，当Y2O3含量小于 10%时 1750烧结材料的维氏硬度比 1700烧结的高，而Y2O3 含量大于 10%时则相反.1750 烧结材料的抗折强度均小于 1700的烧结材料。这可能是因为维氏硬度与Sialon 中的 Y2O3固熔量有关，抗折强度与Sialon 的晶形有关，当Y2O3含量小于 10%时 Sialon 中的Y2O3固熔量随烧结
9、温度的增加而增加，因此 1750烧结材料的维氏硬度比1700烧结材料的高，但Y2O3含量大于 10%时，材料密度对维氏硬度的影响起主要作用，因此1750烧结材料的维氏硬度比1700 烧结材料的低；烧结温度高导致名师资料总结-精品资料欢迎下载-名师精心整理-第 3 页，共 8 页 -Sialon 的棒状晶形减少、粒状晶形增加，因此 1750烧结材料的抗折强度比1700烧结材料的低。当1700烧结时材料的维氏硬度峰值达到13.68GPa、而抗弯强度最高为 237MPa。2.3 材料的组织和物相图 4 为不同 Y2O3 含量的材料在不同烧结温度下的金相组织。由图可知随着 Y2O3含量的增加材料中Si
10、alon 柱状晶的比例在增加（图4a、b 到图 4c、d），随着烧结温度的增加材料中Sialon 等轴晶的比例在增加。这是由于单相 Ca-Sialon通常形成等轴晶体 11，而固溶 Y3+的(Ca/Y)-Sialon则可能形成柱状晶体12-13，烧结温度高可以促进(Ca/Y)-Sialon柱状晶的粗化和等轴化。图4中的白色球形颗粒为Fe4N，烧结温度的增加促进了Fe4N的长大。图为Y2O3含量为 10%材料在不同烧结温度下的XRD 衍射图谱，由图可知，随着烧结温度的增加材料中FeN的衍射峰明显，并逐渐出现出YAG的衍射峰，说明烧结温度促进了 Fe4N的长大，Y2O3和 Al2O3的加入生成了少
11、量的YAG。2.4 材料的断裂特点图 6 为 Y2O3 含量分别为 6%和 10%的材料在 1700烧结后的断口照片。由图可知，两种成分样品均为沿晶断裂，图6a 中比图 6b 存在较多的亚裂纹，也说明Y2O3含量的增加促进了材料的烧结，减少了材料中的亚裂纹，这也是Y2O3 提高材料强度的另一个原因。3 结论名师资料总结-精品资料欢迎下载-名师精心整理-第 4 页，共 8 页 -（1）适量的 Y2O3促进材料的烧结致密化和提高材料的力学性能，但 Y2O3（大于 10%）过量时对材料的烧结和力学性能不利。（2）掺杂 Y3+的(Ca/Y)-Sialon呈柱状晶，随着 Y2O3含量的增加和烧结温度的提
12、高，(Ca/Y)-Sialon呈柱状晶出现粗化和等轴化。（3）含 10Y2O3的材料在 1700烧结时可获得较高的力学性能。名师资料总结-精品资料欢迎下载-名师精心整理-第 5 页，共 8 页 -Construction and properties of(Ca/Y)-Sialon ceramics synthesized from blast furnace water quenching slag XXXXXXX Abstract:Rare-earth composite(Ca/Y)-Sialon ceramics were fabricated using Ca-Sialon power
13、s synthesized from blast furnace water quenching slag.Investigations were carried out to analyze the densification process in sintering,mechanical properties,and microstructure,phase-transformation and fracture characteristics.The results show that a certain amounts of Y2O3additions can promote the
14、densification action of sintering and improve mechanical properties of(Ca/Y)-Sialon ceramics.But the excess amounts of Y2O3（more than 10%）is disadvantaged.In the samples elongated(Ca/Y)-Sialon grains were found and the microstructure changed from elongated to agglomerate with increasing yttrium leve
15、ls.The excellent mechanical properties of(Ca/Y)-Sialon ceramics are obtained when sintering at 1700 with the addition of 10%Y2O3.Keywords:(Ca/Y)-Sialon,water quenching slag,pressureless sintering,mechanical properties,microstructure Blast furnace water quenching slag is a by-product produced in the
16、iron-smelting course.Its main constituent includes SiO2,Al2O3,CaO and some impurity phase of Fe,which mainly used for making cement at present.How to improve added value of blast furnace water quenching slag is the thing that people dream of 1.at present People utilize Blast furnace slag to synthesi
17、s Sialon powder and it already to be carried on extensive research,for instance Liu KeMing 2,etc.have studied that thermodynamics analysis and craft optimization of utilizing Blast furnace slag to synthesis Ca-Sialon,Jiang Tao,etc.3 have studied that processing parameter of utilizing Blast furnace s
18、lag to synthesis Ca-Mg-Sialon,Jiang JiuXin,etc.4 have studied high temperature SHS synthesis craft of slag Ca-Sialon powder.But at present the property of the pressless-sintered Sialon ceramic using Sialon powder synthesis form slag is not good enough,and the craft is complicated,for instance Chen W
19、eiWu,etc.5 utilizes the methods of burying powder pressless-sintered(1800)and the hot-press sintered to get(Ca,Mg)-Sialon ceram.Sialon ceram has fine property,has extensive uses in the structure ceramic,and to be considered one of the most promising structural ceramics 6.But because of the high nitr
20、ogen content of the -Sialon material,there are some difficulties in the pressless-sintering densification of the material.7 After sintering,the metal ion as of additive can enter -Sialon structure to reduce the content of grain boundary phase,and improve the mechanics property of the material.Recent
21、 research indicates that Y2O3 can reduce the ceramic sintering temperature 8.In our work,investigations were carried out to analyze the densification process in sintering,mechanical properties,phase,microstructure of the pressless-sintering(Ca/Y)-Sialon with Ca-Sialon synthesized from slag as raw ma
22、terials,with Al2O3 and Y2O3 as additive.It offers a new way for the use of the slag.1 An experiment course The experiment adopted Ca-Sialon powder synthesis from blast furnace water quenching slag(offered by BaoTian Company of Shanghai,main constituent is Ca-Sialon,Fe4N is the mainly impurity elemen
23、ts,there are also some impurity elements such as Cr,Mo,Mn,etc.)for raw materials,with Al2O3(average grain size is smaller than 1m)and Y2O3(content is 99.9 wt%,average grain size is smaller than 1m)as sintering assistant.The content of Al2O3 is 5%,which of Y2O3 are 4,6,8,10,12 and 14wt%respectively i
24、n the Sample.Confectioning binding admixture is polyvinyl alcohol;add 10%of total quality.Then ball milling the initial powder material according to batch formula and mix 12h.Use alumina as ball grinding ball,the medium is the ethyl alcohol.After the ball milling,the material was dried,prilled,and t
25、hen made a single-phase-pre-extrude under 40MPa pressure(the size of sample is 6*6*36mm),and then cold isostatic compaction under 200MPa.The 名师资料总结-精品资料欢迎下载-名师精心整理-第 6 页，共 8 页 -body dried at 100 for 12h,then sintered under pure N2 atmosphere of 0.1MPa,sintering system adopt 1700 for 1.5h and 1750 fo
26、r 1.5h two kinds of systems respectively.Utilize Archimedes principle to determine the volume density of the sample.Utilize Model D/max-rB X ray diffraction(X-ray diffraction,XRD)to analyze the phase.Adopt the universal material testing machine of Model WD210 electron to measure flexural strength th
27、ree of the material,its load speed is 0.5mm/min.flexural strength value fetches the averages of 5 samples.Use Vickers hardness tester to measure the Vickers hardness of the material,the load is 5kg,fetch the averages of 4 samples.Utilize the Model SSX-550 stereo scan to scan the micro-pattern,and ut
28、ilize EDX to carry on micro-area composition analysis.Adopt GX71 metallographical microscope to analyse the microscopic structure.Utilize LEXT OLS3000 microscope to carry on material fracture behavior analysis.2 results and discussing 2.1 Sintering behavior of different Y2O3 content materials Fig.1
29、shows volume density of the samples varies with Y2O3 content.We can see from the figure,with the increase of Y2O3 content,volume density of the samples reduced after increasing,density of samples of different Y2O3 content sintered in 1750 are lower than that in 1700,the highest volume density of the
30、 material is 3.32g/cm3 as content of Y2O3 content for 10%,temperature of sintering in 1700.On one hand this is because Y3+and O2-ion of Y2O3 is easy to get into Sialon crystal lattice,which will make Sialon crystal lattice distortion 9,on the other hand,Y2O3 and Al2O3 added in and sample forms YAG 1
31、0,thus promoted the sintering behavior of the material,but when Y2O3 content exceeds 10%,the solid solution in Sialon obviously increases,which makes the melting point of Sialon reduce greatly,it is easy to present volatile matter and bubble in the sample,make the density of the sample reduce.When s
32、intering temperature increases,volatile matter and bubble increase too,so the density of the sample is reduced too.2.2 Mechanics performance of the material Fig.2 and Fig.3 shows the influence of Y2O3 content on Vickers hardness and flexural strength respectively.We can see from the figures,Vickers
33、hardness and flexural strength of the samples reduced after increasing with the increase of Y2O3 content,this is the same as law of influence on volume density of material with Y2O3 content(Fig.1),prove that right amount Y2O3 promotes materials to sintered,make the mechanics property of the material
34、 raise,but excess Y2O3 content makes the density of material reduce,so the mechanics property of the material is reduced.We can also see from the figures Fig.2 and Fig.3,influence of sintering temperature on the hardness relate to Y2O3 content,when Y2O3 content below 10%,Vickers hardness is higher s
35、intered in 1750than that in 1700,but when Y2O3 content is over 10%,the situation is opposite.Flexural strength of the sintering materials is lower sintered in 1750 than that in 1700.This may because Vickers hardness is related to Y2O3 solid melting amount in Sialon,while flexural strength is related
36、 to crystals shape of Sialon,Y2O3 solid melting amount in Sialon increase with the sintering temperature increases when Y2O3 content below 10%,so Vickers hardness of material is higher sintered in 1750 than sintered in 1700,when Y2O3 content is over 10%,the influence of material density on hardness
37、is the main one,so Vickers hardness of material is lower sintered in 1750 sintered in than 1700;The numbers of rod like grains of Sialon reduce and equiaxed grains of Sialon increase with high temperature,so flexural strength of material is lower sintered in 1750than sintered in 1700.The peak value
38、of the hardness of the material reaches 13.68GPa;the highest flexural strength is 237MPa when sintered in 1700.2.3 The structure and phase of the material Fig.4 is metallurgical structure photos of material of different Y2O3 content under different sintering temperature.We can see from the figures t
39、hat the rate of Sialon columnar grains of the material increase with Y2O3 content increase(From Fig.4a,b to Fig.4c,d),the rate of Sialon equiaxed grains of the material increase with sintering 名师资料总结-精品资料欢迎下载-名师精心整理-第 7 页，共 8 页 -temperature increase.This is because single-phase Ca-Sialon usually for
40、m equiaxed crystal 11 ,Y3+solid melting(Ca/Y)-Sialon may form columnar crystal12-13,high sintering temperature can promote the microstructure changed from elongated to agglomerated.The white spherical particle in Fig.4 is Fe4N,increase of sintering temperature promoted the growing up of Fe4N.Fig.5 i
41、s X-ray diffraction figure of materials that the Y2O3 content is 10%,sintered at different temperature,We can see from the figure,the diffraction peak of FeN is obvious,and the diffraction peak of YAG appears gradually with the increase of sintering temperature,prove that the increase of sintering t
42、emperature promoted the growing up of Fe4N,the joining of Y2O3 and Al2O3 form a small amount of YAG.2.4 Fracture characteristic of the material Fig.6 photos of fracture of materials which the Y2O3 content is 6%and 10%respectively after sintering in 1700.We can see from the figure,two kinds of compos
43、ition samples are all 沿晶断裂,samples of Fig.6a have more inferior crackle than Fig.6b,prove that the increase of Y2O3 content has promoted the sintering of the material too,has reduced the inferior crackle in materials,this is another reason why Y2O3 improves the intensity of material too.3 conclusion
44、s(1)Right amount Y2O3 promotes the sintering densification process and improve the mechanics property of the material,but it is disadvantageous to sintering of the material and mechanics property when Y2O3 is excessive(over 10%).(2)Y3+dope(Ca/Y)-Sialon is columnar crystals,the columnar crystals of(Ca/Y)-Sialon become.thicker and equiaxed with increase content of Y2O3 and improvement of sintering temperature.(3)The material including 10%Y2O3 can obtain higher mechanics property when sintering at 1700.名师资料总结-精品资料欢迎下载-名师精心整理-第 8 页，共 8 页 -