田口法研究3Y-TZP/TiN导电陶瓷材料最佳化制程

doi:10.3724/SP.J.1077.2012.00529

摘要/Abstract

摘要：

实验用田口法研究了添加30wt%氮化钛的钇稳定氧化锆基陶瓷材料(3Y-TZP/TiN)制造工艺. 选择烧结方式、TiN粉末振荡时间、第一阶段保温时间及第二阶段烧结温度四个工艺参数作为控制因子, 设计L₉正交表进行实验规划. 烧结后, 检测试片断裂韧性、抗弯强度、硬度、相对密度及电阻值. 最后通过变异数分析找出最佳参数, 再进行实验验证. 本研究得到的最佳化烧结工艺为: TiN粉末振动8 h, 采用两步烧结法, 第一阶段烧结温度1450℃, 不保温, 第二阶段烧结温度1150℃, 保温20 h. 结果显示, 采用该工艺得到了抗弯强度平均值为736.75 MPa、断裂韧性为7.545 MPa·m^1/2的氧化锆基导电陶瓷材料. 研究发现, 第一阶段保温时间对断裂韧性的影响程度最大, 其次依次为烧结方式、TiN粒径大小及第二阶段保温温度. 断裂韧性的微结构影响因子为四方相与单斜相数量的比值, 当此值达到最高时, 断裂韧性也达到最高值为9.275 MPa·m^1/2. 另外, 添加30wt% TiN的氧化锆电阻率平均值为3.26 m?·cm, 可以进行电火花加工.

关键词: 钇稳定氧化锆, 田口法, 变异数分析, 抗弯强度, 断裂韧性

Abstract:

For the manufacturing of 3mol% Yttria- tetragonal Zirconia polycrystal (3Y-TZP) with 30wt% of Titanium Nitride (TiN) (3Y-TZP/TiN) powders, Taguchi method was used to selected the process parameters including sintering step variation, crushing time of TiN powder, the first step sintering duration and second step sintering temperature to be the controlling factors. The characterization features of sintered samples such as fracture toughness, flexural strength, hardness, relative density and electric resistance were explored through L₉ orthogonal array. By analysis of variance (ANOVA), the optimal parameter settings for each response factor were obtained and tested through confirmation experiments. The results indicate that the optimal process parameters contain 8 h crushing time of TiN powder, two - steps sintering processes including the 1450℃ temperature with no duration for the first step and 1150℃ temperature and 20 h duration for the second step, and the average flexural strength of 736.75 MPa and fracture toughness of 7.545 MPa•m^1/2 are obtained. In addition, the degree of the process parameter effects on the sintered samples is found in the series of the sintering duration of the first step, sintering step variation, size of TiN particles and the sintering temperature of the second step. Meanwhile, fracture toughness depends significantly on the ratio of tetragonal phase to monoclinic phase and attends to be 9.275 MPa·m^1/2 when the ratio is getting to the maximum. The average electric resistance for 3Y- TZP/ TiN is measured to be 3.26 m?·cm. These samples can be electric-discharge machined.

Key words: 3mol% Yttria-tetragonal zirconia (3Y-TZP), Taguchi method, analysis of variance(ANOVA), flexural strength, fracture toughness

中图分类号:

TQ174

王翠凤 , 邱锡荣, 欧耿良, 蔡长庭. 田口法研究3Y-TZP/TiN导电陶瓷材料最佳化制程[J]. 无机材料学报, 2012, 27(5): 529-535.

WANG Cui-Feng, CHIOU Shi-Yung, OU Keng-Liang, CAI Zhang-Ting. Optimal Process Parameters for 3Y-TZP/TiN Conductive Polycrystal by Taguchi Method[J]. Journal of Inorganic Materials, 2012, 27(5): 529-535.

图/表 12

参考文献 16

[1]	Shi J L, Li B S, Lu Z L, et al. Correlation between microstructure, phase transformation during fracture and the mechanical properties of Y-TZP Ceramics. Journal of the European Ceramic Society, 1996, 16(7): 795-798.
[2]	Jansen S R, Winnubst A J A, He Y J, et al. Effects of grain size and ceria addition on ageing behaviour and tribological properties of Y-TZP ceramics. Journal of the European Ceramic Society, 1998, 18(5): 557-563.
[3]	Tseng Wenjea J, Taniguchi Masahiko, Yamada Toshiyuki. Transformation strengthening of as-fired zirconia ceramics. Ceramics International, 1999, 25: 545-550.
[4]	Vanmeensel K, Laptev A, Van der Biest O, et al. The influence of percolation during pulsed electric current sintering of ZrO2–TiN powder compacts with varying TiN content. Acta Materialia, 2007, 55(5):1801–1811.
[5]	Bonny K, De Baets P, Vleugels J, et al. Influence of secondary electro-conductive phases on the electrical discharge machinability and frictional behavior of ZrO2-based ceramic composites. Journal of Materials Processing Technology, 2008, 208(1/2/3): 423-430.
[6]	Lauwers B, Brans K, Liu W, et al. Influence of the type and grain size of the electro-conductive phase on the Wire-EDM performance of ZrO2 ceramic composites. CIRP Annals - Manufacturing Technology, 2008, 57(1): 191-194.
[7]	王光国. 氮化钛对钇安定化氧化锆性能与组织之影响. 台湾高雄: 国立高雄应用科技大学硕士论文, 2005.
[8]	Puertas I, Luis C J. A study on the electrical discharge machining of conductive ceramics. Journal of Materials Processing Technology, 2004, 153–154:1033-1038.
[9]	Perez Delgado Y, Bonny K, De Baets P, et al. Impact of wire-EDM on dry sliding friction and wear of WC-based and ZrO2-based composites. Wear, 2011, 271(9/10):1951-1961.
[10]	Lauwers B, Kruth J P, Liu W, et al. Investigation of material removal mechanisms in EDM of composite ceramic materials. Journal of Materials ProcessingTechnology, 2004, 149(1/2/3): 347-352.
[11]	Alfonso Bravo-Leon, Yuichiro Morikawa, Masanori Kawahara, et al. Fracture toughness of nanocrystalline tetragonal zirconia with low yttria content. Acta Materialia, 2002, 50(18): 4555-4562.
[12]	Shibata Kenro, Sato Rikiya, Yoshinaka Masaru, et al. Electrical and mechanical properties of ZrO2(2Y)/TiN composites and laminates made from these materials. Journal of Materials Science, 1997, 32(3): 583-587.
[13]	Ran Songlin, Gao Lian. Mechanical properties and microstructure of TiN/TZP nanocomposites. Materials Science and Engineering A, 2007, 447(1/2): 83-86.
[14]	Jef Vleugels, Omer Van der Biest. Development and characterization of Y2O3-Stabilized ZrO2 (Y-TZP) Composites with TiB2, TiN, TiC, and TiC0.5N0.5. Journal of the American Ceramic Society, 1999, 82(10): 2717-2720.
[15]	Bonny K, De Baets P, Ost W, et al. Influence of secondary phases on the tribological response of electro-discharge machined zirconia- based composites against WC-Co cemented carbide. Wear, 2009, 267(12): 2157-2166.
[16]	Lopez-Esteban S, Gutierrez-Gonzalez C F, Mata-Osoro G, et al. Electrical discharge machining of ceramic/semiconductor/metal nanocomposites. Scripta Materialia, 2010, 63(2): 219-222.

Experiment	Sintering type	TiN crushing time/h	Duration time for the first step/h	Sinter temperature for the second step/℃
Exp.1	Conventional sintering(no duration time for the second step)	4	2	-
Exp.2	Conventional sintering(no duration time for the second step)	8	1	-
Exp.3	Conventional sintering(no duration time for the second step)	12	0	-
Exp.4	Two steps sintering(10 h duration time for the second step)	4	1	1050
Exp.5	Two steps sintering(10 h duration time for the second step)	8	0	1250
Exp.6	Two steps sintering(10 h duration time for the second step)	12	2	1150
Exp.7	Two steps sintering(20 h duration time for the second step)	4	0	1150
Exp.8	Two steps sintering(20 h duration time for the second step)	8	2	1050
Exp.9	Two steps sintering(20 h duration time for the second step)	12	1	1250

Experiment	Sintering type	TiN crushing time/h	Duration time for the first step/h	Sinter temperature for the second step/℃
Exp.1	Conventional sintering(no duration time for the second step)	4	2	-
Exp.2	Conventional sintering(no duration time for the second step)	8	1	-
Exp.3	Conventional sintering(no duration time for the second step)	12	0	-
Exp.4	Two steps sintering(10 h duration time for the second step)	4	1	1050
Exp.5	Two steps sintering(10 h duration time for the second step)	8	0	1250
Exp.6	Two steps sintering(10 h duration time for the second step)	12	2	1150
Exp.7	Two steps sintering(20 h duration time for the second step)	4	0	1150
Exp.8	Two steps sintering(20 h duration time for the second step)	8	2	1050
Exp.9	Two steps sintering(20 h duration time for the second step)	12	1	1250

Crushing time	Particle size /%	Particle size /percentage	Particle size /percentage	Particle size /percentage
4 h	0.303 /40%	0.991/24%	3.535/36%	-
8 h	0.293/45%	1.002 /21%	3.043/12%	9.837/22%
12 h	0.264 /53%	0.954/16%	5.588/31%	-

Crushing time	Particle size /%	Particle size /percentage	Particle size /percentage	Particle size /percentage
4 h	0.303 /40%	0.991/24%	3.535/36%	-
8 h	0.293/45%	1.002 /21%	3.043/12%	9.837/22%
12 h	0.264 /53%	0.954/16%	5.588/31%	-

Experiment	Flexural strength/MPa	Fracture toughness/(MPa·m^1/2)
Exp.1	602.437	4.055
Exp.2	648.402	5.215
Exp.3	574.059	6.340
Exp.4	738.188	5.180
Exp.5	732.302	9.275
Exp.6	739.225	4.800
Exp.7	742.437	7.545
Exp.8	749.450	5.765
Exp.9	790.125	6.415