Ti/C_(0.36)N_(0.64)为原料合成Ti(C,N)及相关化合物的研究
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摘要
本论文采用三聚氰胺热解物固态(C_(0.36)N_(0.64))粉末为碳和氮源，通过燃烧合成法和机械合金化法及放电等离子烧结技术，制备了Ti(C,N)化合物及相关材料，并系统地研究了其形成机制和基本理化特性。
借助于三聚氰胺热解法制备了一种具有乱层石墨结构的固态碳氮(C_(0.36)N_(0.64))粉末，其成分为36.0at%C、63.5at%N和0.5at%H，不含O等杂质元素；热分析表明该碳氮粉末分解温度为600~800℃。该碳氮粉末是制备Ti(C,N)的理想固态氮源和碳源。
采用Ti和(C_(0.36)N_(0.64))粉末为原料，探索了热爆反应合成Ti(C,N)化合物的可行性，结果表明产物中Ti(C,N)含量较低。分析认为是由于热爆反应速率较低，且反应体系处于开放空间，使(C_(0.36)N_(0.64))粉末挥发严重，导致合成产物中Ti(C,N)较少。利用化学炉法引发的二次热爆过程可促进Ti(C,N)的形成，获得的合成产物主相为Ti(C,N)和TiN。
利用自蔓延高温反应法(SHS)，以Ti/C_(0.36)N_(0.64)为原料成功制备了纯相的Ti(C_(0.30)N_(0.70))化合物粉末，粉体的平均粒径为3μm。采用淬熄技术系统研究了Ti(C,N)化合物的SHS法形成机理，结果表明：随温度升高C_(0.36)N_(0.64)粉末分解形成N2和C2N2等气体，进而Ti与N2反应生成TiN和Ti_2N，过程中放出大量的热，促使大量的Ti与C2N2反应生成Ti(C,N),以及前期生成的Ti_2N和TiN或Ti与C_(0.36)N_(0.64)粉末直接反应，生成Ti(C,N)。各种反应交织进行，最后获得单相的Ti(C,N)。分别采用SHS和热爆两种方法，研究了Al/C_(0.36)N_(0.64)、V/C_(0.36)N_(0.64)和Ti/Al/C_(0.36)N_(0.64)
体系的反应过程。SHS研究表明：Al/C_(0.36)N_(0.64)和V/C_(0.36)N_(0.64)体系可以分别获得三元铝碳氮和V(C,N)。Ti/Al/C_(0.36)N_(0.64)体系产物为Ti_2Al(C,N)-Ti_(19)Al_(16)，Ti3Al(C,N)2-Ti(C,N)和AlN-Ti(C,N)等复合化合物；利用热爆法对Al/C_(0.36)N_(0.64)和Ti/Al/C_(0.36)N_(0.64)体系处理，其产物分别以AlN和Ti_2Al(C,N)-TiAl为主相。采用放电等离子热压烧结（SPS）法制备了Ti(C,N)，研究结果表明：SPS合成
Ti(C,N)的反应路径为：Ti+C_(0.36)N_(0.64)→Ti过饱和固溶体→TiC+TiN→Ti(C,N)以及Ti+C_(0.36)N_(0.64)→Ti过饱和固溶体→Ti(C,N)。通过机械球磨法(MA)，以Ti/C_(0.36)N_(0.64)为原料成功制备出纳米Ti(C,N),利用获得
的纳米Ti(C,N)进行SPS烧结，在1600℃得到致密度98%的细晶Ti(C,N)块体材料，其硬度和抗折强度分别为17GPa和700MPa。
利用C0.36N0.64粉末、Ti和Al粉作为结合剂，以热爆烧结法成功制备出包含20%金刚石或c-BN的，以TiAl-Ti_2Al(C,N)为基的致密复合块体材料，微观形貌观察表明金刚石或c-BN晶粒与TiAl-Ti_2Al(C,N)基体结合紧密，为进一步开发新型超硬材料工具提供了参考。
In this paper, we discussed the preparation of the Ti (C, N) compound and the relevant materials by combustion synthesis, mechanical alloying and spark plasma sintering, adopting the solid carbon and nitrogen precursor (C0.36N0.64) powder as the carbon and nitrogen source. We also studied the formation mechanism of the material and its basic physical and chemical properties in a systematic way.
Using melamine pyrolysis method, a solid state carbon and nitrogen (C0.36N0.64) powders with a turbostratic graphite structure were obtained, which had a composition of36.0at%C,63.5at%N and0.5at%H. Thermal analysis indicated that the decomposition temperature of this carbon and nitrogen powders were between600-800℃. Therefore, these carbon-nitrogen powders are the ideal nitrogen and carbon sources for the preparation of Ti (C, N).
Applying Ti and (C0.36N0.64) powders as raw materials, we explored the feasibility of synthesizing Ti (C, N) compound by thermal explosion reaction. The result showed that the content of Ti (C, N) was low in the resulting product. Analysis considered that the thermal explosion reaction rate was low, and the reaction system was in the open space, leading to a serious volatilization of the (C0.36N0.64) powder, resulting in the less Ti (C, N) in the composition. Utilizing the secondary thermal explosion process that formed during the chemical furnace method, it may promote the formation of Ti (C, N). The main phases of the obtained synthetic products were Ti (C, N) and TiN.
The powder of the pure phase Ti (C0.30N0.70) compound was successfully prepared, utilizing the self-propagating high-temperature reaction (SHS), with Ti/Co.36No.64as the raw material. The average particle size of the powder was3μm. The synthetic mechanism of the Ti (C, N) compound was studied systematically by quenching technique. The results showed that before the decomposition of Co.36No.64powder occurred, it had already reacted with Ti in a solid-solid reaction, and formed a small amount of TiN and TiC. As the temperature increasing, Co.36No.64powder decomposed to gases such as N2and C2N2, and then Ti reacted with N2and formed TiN and Ti2N. During this process, a considerable amount of heat were released, prompting a large amount of Ti reacted with C2N2, formed Ti (C, N). Along with the formed TiN and Ti2N, a direct reaction with Co.36No.64powder took place. Eventually the pure phase of Ti (C0.30N0.70) formed.
The two methods SHS and thermal explosion were used respectively to research the reaction processes of the Al/Co.36No.64, V/Co.36No.64and Ti/Al/Co.36No.64systems. SHS studies indicated that the Al/Co.36No.64and V/C0.36N0.64systems could obtain the ternary aluminum, carbon and nitrogen and V(C, N), respectively. The Ti/Al/C0.36N0.64system products were Ti2Al(C, N)-Ti3Al, Ti3Al(C, N)2-TiC and AlN-Ti(C, N), and other complex compounds. To treat the Al/Co.36No.64and Ti/Al/Co.36No.64system by thermal explosion reaction, a main phase of A1N and Ti2Al(C, N)-TiAl in the formed products were achieved, respectively.
The Ti (C, N) were prepared by spark plasma sintering (SPS). The results indicated that the synthetic route of Ti (C, N) with SPS was Ti+C0.36N0.64→Ti supersaturated solid solution→TiC+TiN→Ti (C, N).
The nano-Ti (C, N) were achieved successfully by mechanical milling method (MA), with Ti/Co.36No.64as raw materials. Using the obtained nano-Ti (C, N) to conduct the SPS sintering, a density of98%fine-grained Ti (C, N) bulk material was obtained at1600℃The mechanical analysis showed the hardness and flexural strength of the material were17GPa and700MPa, respectively.
Using C0.36N0.64powder, titanium and aluminum as a binder, a dense composite bulk material, containing20%of the diamond or cubic boron nitride of TiAl-Ti2Al(C,N) were prepared successfully by thermal explosion sintering. The observed micro-morphology indicated that the diamond or cubic boron nitride grains bound with the TiAl-Ti2Al(C,N) base together tightly, which will establish the theoretical foundation for the further development of the new tools of super-hard materials.
借助于三聚氰胺热解法制备了一种具有乱层石墨结构的固态碳氮(C_(0.36)N_(0.64))粉末，其成分为36.0at%C、63.5at%N和0.5at%H，不含O等杂质元素；热分析表明该碳氮粉末分解温度为600~800℃。该碳氮粉末是制备Ti(C,N)的理想固态氮源和碳源。
采用Ti和(C_(0.36)N_(0.64))粉末为原料，探索了热爆反应合成Ti(C,N)化合物的可行性，结果表明产物中Ti(C,N)含量较低。分析认为是由于热爆反应速率较低，且反应体系处于开放空间，使(C_(0.36)N_(0.64))粉末挥发严重，导致合成产物中Ti(C,N)较少。利用化学炉法引发的二次热爆过程可促进Ti(C,N)的形成，获得的合成产物主相为Ti(C,N)和TiN。
利用自蔓延高温反应法(SHS)，以Ti/C_(0.36)N_(0.64)为原料成功制备了纯相的Ti(C_(0.30)N_(0.70))化合物粉末，粉体的平均粒径为3μm。采用淬熄技术系统研究了Ti(C,N)化合物的SHS法形成机理，结果表明：随温度升高C_(0.36)N_(0.64)粉末分解形成N2和C2N2等气体，进而Ti与N2反应生成TiN和Ti_2N，过程中放出大量的热，促使大量的Ti与C2N2反应生成Ti(C,N),以及前期生成的Ti_2N和TiN或Ti与C_(0.36)N_(0.64)粉末直接反应，生成Ti(C,N)。各种反应交织进行，最后获得单相的Ti(C,N)。分别采用SHS和热爆两种方法，研究了Al/C_(0.36)N_(0.64)、V/C_(0.36)N_(0.64)和Ti/Al/C_(0.36)N_(0.64)
体系的反应过程。SHS研究表明：Al/C_(0.36)N_(0.64)和V/C_(0.36)N_(0.64)体系可以分别获得三元铝碳氮和V(C,N)。Ti/Al/C_(0.36)N_(0.64)体系产物为Ti_2Al(C,N)-Ti_(19)Al_(16)，Ti3Al(C,N)2-Ti(C,N)和AlN-Ti(C,N)等复合化合物；利用热爆法对Al/C_(0.36)N_(0.64)和Ti/Al/C_(0.36)N_(0.64)体系处理，其产物分别以AlN和Ti_2Al(C,N)-TiAl为主相。采用放电等离子热压烧结（SPS）法制备了Ti(C,N)，研究结果表明：SPS合成
Ti(C,N)的反应路径为：Ti+C_(0.36)N_(0.64)→Ti过饱和固溶体→TiC+TiN→Ti(C,N)以及Ti+C_(0.36)N_(0.64)→Ti过饱和固溶体→Ti(C,N)。通过机械球磨法(MA)，以Ti/C_(0.36)N_(0.64)为原料成功制备出纳米Ti(C,N),利用获得
的纳米Ti(C,N)进行SPS烧结，在1600℃得到致密度98%的细晶Ti(C,N)块体材料，其硬度和抗折强度分别为17GPa和700MPa。
利用C0.36N0.64粉末、Ti和Al粉作为结合剂，以热爆烧结法成功制备出包含20%金刚石或c-BN的，以TiAl-Ti_2Al(C,N)为基的致密复合块体材料，微观形貌观察表明金刚石或c-BN晶粒与TiAl-Ti_2Al(C,N)基体结合紧密，为进一步开发新型超硬材料工具提供了参考。
In this paper, we discussed the preparation of the Ti (C, N) compound and the relevant materials by combustion synthesis, mechanical alloying and spark plasma sintering, adopting the solid carbon and nitrogen precursor (C0.36N0.64) powder as the carbon and nitrogen source. We also studied the formation mechanism of the material and its basic physical and chemical properties in a systematic way.
Using melamine pyrolysis method, a solid state carbon and nitrogen (C0.36N0.64) powders with a turbostratic graphite structure were obtained, which had a composition of36.0at%C,63.5at%N and0.5at%H. Thermal analysis indicated that the decomposition temperature of this carbon and nitrogen powders were between600-800℃. Therefore, these carbon-nitrogen powders are the ideal nitrogen and carbon sources for the preparation of Ti (C, N).
Applying Ti and (C0.36N0.64) powders as raw materials, we explored the feasibility of synthesizing Ti (C, N) compound by thermal explosion reaction. The result showed that the content of Ti (C, N) was low in the resulting product. Analysis considered that the thermal explosion reaction rate was low, and the reaction system was in the open space, leading to a serious volatilization of the (C0.36N0.64) powder, resulting in the less Ti (C, N) in the composition. Utilizing the secondary thermal explosion process that formed during the chemical furnace method, it may promote the formation of Ti (C, N). The main phases of the obtained synthetic products were Ti (C, N) and TiN.
The powder of the pure phase Ti (C0.30N0.70) compound was successfully prepared, utilizing the self-propagating high-temperature reaction (SHS), with Ti/Co.36No.64as the raw material. The average particle size of the powder was3μm. The synthetic mechanism of the Ti (C, N) compound was studied systematically by quenching technique. The results showed that before the decomposition of Co.36No.64powder occurred, it had already reacted with Ti in a solid-solid reaction, and formed a small amount of TiN and TiC. As the temperature increasing, Co.36No.64powder decomposed to gases such as N2and C2N2, and then Ti reacted with N2and formed TiN and Ti2N. During this process, a considerable amount of heat were released, prompting a large amount of Ti reacted with C2N2, formed Ti (C, N). Along with the formed TiN and Ti2N, a direct reaction with Co.36No.64powder took place. Eventually the pure phase of Ti (C0.30N0.70) formed.
The two methods SHS and thermal explosion were used respectively to research the reaction processes of the Al/Co.36No.64, V/Co.36No.64and Ti/Al/Co.36No.64systems. SHS studies indicated that the Al/Co.36No.64and V/C0.36N0.64systems could obtain the ternary aluminum, carbon and nitrogen and V(C, N), respectively. The Ti/Al/C0.36N0.64system products were Ti2Al(C, N)-Ti3Al, Ti3Al(C, N)2-TiC and AlN-Ti(C, N), and other complex compounds. To treat the Al/Co.36No.64and Ti/Al/Co.36No.64system by thermal explosion reaction, a main phase of A1N and Ti2Al(C, N)-TiAl in the formed products were achieved, respectively.
The Ti (C, N) were prepared by spark plasma sintering (SPS). The results indicated that the synthetic route of Ti (C, N) with SPS was Ti+C0.36N0.64→Ti supersaturated solid solution→TiC+TiN→Ti (C, N).
The nano-Ti (C, N) were achieved successfully by mechanical milling method (MA), with Ti/Co.36No.64as raw materials. Using the obtained nano-Ti (C, N) to conduct the SPS sintering, a density of98%fine-grained Ti (C, N) bulk material was obtained at1600℃The mechanical analysis showed the hardness and flexural strength of the material were17GPa and700MPa, respectively.
Using C0.36N0.64powder, titanium and aluminum as a binder, a dense composite bulk material, containing20%of the diamond or cubic boron nitride of TiAl-Ti2Al(C,N) were prepared successfully by thermal explosion sintering. The observed micro-morphology indicated that the diamond or cubic boron nitride grains bound with the TiAl-Ti2Al(C,N) base together tightly, which will establish the theoretical foundation for the further development of the new tools of super-hard materials.
引文
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