High-Pressure and High-Temperature Sintering of Bulk Tungsten and W-TiC Alloy with Near-Full Densification and High Hardness
-
摘要: 采用高温高压烧结方法,烧结纯钨和TiC颗粒弥散增强W-TiC合金材料,对钨及W-TiC合金的烧结致密化行为和力学性能进行了研究。结果表明:在压力为5.0 GPa、温度为1 500 ℃的条件下烧结15 min可获得良好的烧结样品,块体钨的致密度达到99.3%,硬度达到6.43 GPa;在相同的高温高压烧结条件下,添加质量分数为1.5%的TiC,获得的W-TiC合金致密度达到99.0%,硬度达到7.58 GPa。极端高压环境不但能抑制钨及钨合金在烧结过程中的晶粒长大,还能降低烧结温度,提高烧结效率,增加烧结体的致密性。在此基础上进一步探索了钨及钨基合金W-TiC的高压烧结动力学、微观结构、机械性能与烧结压力和烧结温度的关系。Abstract: The pure bulk tungsten and W-TiC alloy were sintered by high-pressure and high-temperature (HPHT) method, and their densification behavior and hardness were systematically investigated.It is found that the pure tungsten sample sintered at the circumstance of 5.0 GPa and 1 500 ℃ for 15 min exhibits unique properties, its relative density and hardness are as high as 99.3% and 6.43 GPa, respectively.Moreover, the values for W-TiC alloy with TiC mass fraction of 1.5% are 99.0% and 7.58 GPa respectively under the same sintering conditions.It is concluded from the experimental results that the HPHT sintering method plays an important role in the aspects of accelerating the densification, improving the sintering efficiency and bringing down the sintering temperature.Furthermore, the relations of the sintering kinetics, microstructures and the evolutions of mechanical properties versus pressure and temperature were all explored for tungsten and W-TiC alloy.
-
Key words:
- tungsten /
- W-TiC /
- densification /
- hardness /
- high pressure /
- grain size
-
表 1 氢气还原处理的纯钨烧结样品的性能
Table 1. Properties of sintered pure tungsten samples by a hydrogen reduction treatment
Temperature/(℃) Pressure/(GPa) Time/(min) Relative density/(%) Hv/(GPa) 1 200 5.0 15 99.1±0.2 5.89 1 300 5.0 15 99.1±0.2 6.06 1 300 5.0 30 99.2±0.2 6.19 1 500 5.0 15 99.3±0.2 6.43 表 2 采用高温高压烧结方法制备的W-1.5%TiC合金性能
Table 2. Properties of W-1.5%TiC alloys sintered by high-pressure and high-temperature method
Temperature/(℃) Pressure/(GPa) Time/(min) Relative density/(%) Hv/(GPa) 1 200 5.0 15 98.2±0.2 6.55 1 300 5.0 15 98.5±0.2 7.14 1 300 5.0 30 98.6±0.2 7.42 1 500 5.0 15 99.0±0.2 7.58 -
[1] 周宇松, 吴希俊, 李冰寒, 等.采用真空热压技术制备纳米金属钨块体材料[J].高压物理学报, 2000, 14(3): 219-223. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=gywlxb200003011Zhou Y S, Wu X J, Li B H, et al. Synthesis of bulk samples of nanorystalline tungsten[J]. Chinese Journal of High Pressure Physics, 2000, 14(3): 219-223. (in Chinese) http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=gywlxb200003011 [2] 黄波, 杨吉军, 唐军, 等.聚变堆面向等离子体钨基材料的研究进展[J].核动力工程, 2012(增2): 101-106. http://www.cqvip.com/QK/95572X/2012S2/1003444539.html [3] Gruber O, Sips A C C, Dux R, et al. Compatibility of ITER scenarios with full tungsten wall in ASDEX Upgrade[J]. Nucl Fusion, 2009, 49(11): 115014. doi: 10.1088/0029-5515/49/11/115014 [4] Li W Y, Zhang Y, Zhou H B, et al. Stress effects on stability and diffusion of H in W: A first-principles study[J]. Nucl Instrum Methods Phys Res Sect B, 2011, 269(14): 1731-1734. doi: 10.1016/j.nimb.2010.12.027 [5] Prabhu G, Chakraborty A, Sarma B. Microwave sintering of tungsten[J]. Int J Refract Met Hard Mater, 2009, 27(3): 545-548. doi: 10.1016/j.ijrmhm.2008.07.001 [6] Gao Z, Viola G, Milsom B, et al. Kinetics of densification and grain growth of pure tungsten during spark plasma sintering[J]. Metall Mater Trans B, 2012, 43(6): 1608-1614. doi: 10.1007/s11663-012-9704-9 [7] Zhou Z, Ma Y, Du J, et al. Fabrication and characterization of ultra-fine grained tungsten by resistance sintering under ultra-high pressure[J]. Mater Sci Eng A, 2009, 505(1): 131-135. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=ae796f33560968f7d8c130d0079299a4 [8] Wang H T, Fang Z Z, Hwang K S, et al. Sinter-ability of nanocrystalline tungsten powder[J]. Int J Refract Met Hard Mater, 2010, 28(2): 312-316. doi: 10.1016/j.ijrmhm.2009.11.003 [9] Yih S W H, Wang C T. Tungsten: Sources, Metallurgy, Properties, and Applications[M]. New York: Plenum Press, 1979. [10] Jain M, Skandan G, Martin K, et al. Microwave sintering: A new approach to fine-grain tungsten-Ⅰ[J]. Int J Powder Metall, 2006, 42(2): 45-50. http://www.researchgate.net/publication/292329763_Microwave_sintering_A_new_approach_to_fine-grain_tungsten-I [11] 谈军, 周张健, 屈丹丹, 等.放电等离子烧结制备超细晶粒W-TiC复合材料[J].稀有金属材料与工程, 2011, 40(11): 1990-1993. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=xyjsclygc201111023Tan J, Zhou Z J, Qu D D, et al. Fabrication of ultra fine grained W-TiC composites by spark plasma sintering[J]. Rare Metal Materials and Engineering, 2011, 40(11): 1990-1993. (in Chinese) http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=xyjsclygc201111023 [12] 种法力, 于福文, 陈俊凌. W-TiC合金面对等离子体材料及其电子束热负荷实验研究[J].稀有金属材料与工程, 2010, 39(4): 750-752. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=xyjsclygc201004042Chong F L, Yu F W, Chen J L. W-TiC alloy plasma facing materials and heat flux performance test under electron beam facility[J]. Rare Metal Materials and Engineering, 2010, 39(4): 750-752. (in Chinese) http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=xyjsclygc201004042 [13] 郭双全, 葛昌纯, 周张健, 等.聚变堆装置中面向等离子体材料钨涂层的研究进展[J].材料导报, 2010, 24(2): 93-97. http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=cldb201003020Guo S Q, Ge C C, Zhou Z J, et al. Research development of tungsten coatings used as plasma facing materials for fusion reactor[J]. Materials Review, 2010, 24(2): 93-97. (in Chinese) http://www.wanfangdata.com.cn/details/detail.do?_type=perio&id=cldb201003020 [14] 张文凯, 彭放, 郭振堂, 等.高压烧结镀Cr、Ti膜金刚石/铜复合材料热导率研究[J].高压物理学报, 2012, 26(3): 306-312. http://www.cqvip.com/QK/96553X/20123/42503279.htmlZhang W K, Peng F, Guo Z T, et al. Research on thermal conductivity of diamond with Cr, Ti coating/copper composite materials by sintering under high pressure[J]. Chinese Journal of High Pressure Physics, 2012, 26(3): 306-312. (in Chinese) http://www.cqvip.com/QK/96553X/20123/42503279.html [15] Liu P P, Peng F, Liu F M, et al. High-pressure preparation of bulk tungsten material with near-full densification and high fracture toughness[J]. Int J Refract Met Hard Mater, 2014, 42: 47-50. doi: 10.1016/j.ijrmhm.2013.10.009 [16] Genc A, Coskun S, Ovecoglu M L. Decarburization of TiC in Ni activated sintered W-x TiC(x=0, 5, 10, 15 wt%)composites and the effects of heat treatment on the microstructural and physical properties[J]. Int J Refract Met Hard Mater, 2010, 28(3): 451-458. doi: 10.1016/j.ijrmhm.2010.02.004 [17] Segurado J, Gonzalez C, Llorca J. A numerical investigation of the effect of particle clustering on the mechanical properties of composites[J]. Acta Mater, 2003, 51(8): 2355-2369. doi: 10.1016/S1359-6454(03)00043-0