TiC基纳米多层膜的微结构和超硬效应
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摘要
纳米多层膜可因超硬效应获得高硬度，材料组合的多样性则可使这类材料同时兼具优异的综合性能。早期具有超硬效应的纳米多层膜主要由两种晶体氮化物组成。基于模板效应的非晶晶化技术路线，不同种类的非晶材料已被用于高硬度的纳米多层膜，然而作为晶体模板层的调制层仍主要由氮化物组成，较少涉及晶体态的碳化物、硼化物或氧化物，材料体系的拓展仍是高硬度纳米多层膜研究的重要方面。
为将高硬度纳米多层膜的材料体系由氮化物基拓展至碳化物基。论文在研究TiC薄膜制备技术的基础上，设计并制备了TiC与立方结构氮化物组成TiC/TiN纳米多层膜、混合结构碳化物组成TiC/WC纳米多层膜、非晶氮化物、碳化物组成TiC/Si_3N_4和TiC/SiC纳米多层膜、以及可反应碳化物组成TiC/B_4C纳米多层膜。研究了这些不同类型纳米多层膜的微结构和力学性能，并进一步揭示了纳米多层膜调制结构对其力学性能影响规律。
论文的主要结论如下：
1、采用反应溅射制备TiC薄膜时，通过调节C_2H_2分压可以控制TiC薄膜的成分、相组成、微结构和力学性能，合适的C_2H_2分压下可获得结晶好、硬度高的单相TiC薄膜，实验获得TiC薄膜最高硬度为31.6GPa。采用化合物靶溅射制备TiC时，薄膜的沉积速率、微结构、化学成分及力学性能皆受基片温度和溅射气压（Ar）的影响。其中溅射气压的影响较为明显，而基片温度在150℃-450℃间时对TiC薄膜结晶性能和硬度的影响有限。
陶瓷靶溅射制备TiC薄膜中，在TiC靶中增加Ti含量形成的富Ti靶(Ti:C=11:9)可获得结晶良好的单相TiC薄膜；化学计量比的TiC靶由于其成分处于相图TiC+C两相区，游离的C原子降低了薄膜的结晶程度和力学性能；而高富Ti的TiC靶（Ti:C=2:1）所得薄膜因产生Ti相而形成Ti+TiC两相结构。由于可避免反应溅射中反应气体与其他组成物的反应，采用富Ti的TiC靶(Ti:C=11:9)的直接溅射法更有益于与其他材料匹配制备纳米多层膜。
2、对由TiN分别与富钛和化学计量比的TiC靶制备的同晶体结构TiC_(0.8)/TiN和TiC_(1.0)/TiN纳米多层膜的研究发现，TiC_(0.8)/TiN纳米多层膜形成的共格外延生长结构可保持至14.4nm的调制周期，并获得最高硬度为38.6GPa的超硬效应。而TiC_(1.0)/TiN纳米多层膜虽也可在3.0nm的调制周期下获得共格外延生长结构，并获得超硬效应，但其最高硬度仅为30.9GPa。这一对比性结果揭示了组成物调制层的结晶状态对纳米多层膜的共格结构和超硬效应的重要影响。
3、对TiC与混合结构WC组成的TiC/WC纳米多层膜的研究表明，在TiC调制层的模板作用下，且WC层厚度小于约1.2nm时，多层膜将形成共格外延生长结构，此时WC层形成与TiC完全相同的立方结构调制层，多层膜的晶体完整性也因互促效应而得到显著提高，并在lWC=0.5nm时获得41.5GPa的最高硬度。当WC层因厚度的进一步增加时，其又转变为以混合结构形式生长，因而破坏了多层膜的共格外延结构，与其对应的多层膜硬度也随之降低。
4、在TiC与非晶态的Si_3N_4和SiC组成TiC/Si_3N_4、TiC/SiC的纳米多层膜中，由于TiC模板层作用，非晶态的SiC和Si_3N_4层均在厚度较薄时（约0.5nm）被晶化为与TiC相同的立方结构并与TiC层共格外延生长，两类多层膜都取得了硬度增高的超硬效应（其最高硬度分别为36.9GPa和37.0GPa）。随着SiC层和Si_3N_4层厚度的增加，多层膜的共格结构逐渐遭到破坏，硬度也逐渐降低。
5、对具有界面反应的TiC/B_4C纳米多层膜的研究发现，B_4C层在厚度约为0.5nm时全部反应生成TiB_2的调制层，多层膜转变为具有共格生长的TiCx/TiB_2纳米多层膜，并获得硬度异常增高的超硬效应，最高硬度达到40GPa。当B_4C调制层厚度进一步增加时，多层膜的共格外延生长结构因存在剩余未参与反应的非晶B_4C调制层而被破坏，多层膜形成TiCx/TiB_2/B_4C的三层结构，其硬度则相应显著降低。并基于实验结果提出了两调制层具有界面反应特征纳米多层膜获得超硬效应的设计要点：1、组成纳米多层膜的两调制层中至少一层需为晶体层，以作为界面反应层晶体生长的模板层；2、另一调制层（可为非晶层）的厚度应较小（≤1nm），以使其能够通过界面反应全部形成新的调制层；3、界面反应生成物与晶体模板层间应不具互溶性，以获得明锐的层间界面；4、较厚的晶体模板层应具有较大的固溶度，以能够吸收反应生成物中多余的游离原子。
6、对TiC/TiN纳米多层膜调制结构参数与力学性能关系的研究表明，只有当纳米多层膜的调制周期和各调制层的厚度均较小，调制层形成了清晰界面的层状结构并具有共格外延生长的结构特征时，多层膜才能产生硬度异常升高的超硬效应；而随调制结构参数的改变，减少调制层厚度将导致多层膜的界面混合区比例增大,增大调制层厚度则使界面数量减少，共格外延生长结构也会遭到破坏，这些结构的改变都使纳米多层膜的硬度明显降低。本文所建立的纳米多层膜调制结构参数与硬度的关系图可为纳米多层膜获得超硬效应的设计提供参考和借鉴。
基于以上研究结果，论文获得了一批具有超硬效应TiC基纳米多层膜的新体系；揭示了调制层结晶状态对纳米多层膜结构和超硬效应的影响规律；提出了具有界面反应的纳米多层膜体系材料和结构设计的要点；提出了纳米多层膜调制结构设计图。
The superhardness effect and diverse material combinations endowthe nanomultilayers with both high hardness and splendidcomprehensive properties. Widening the system of hard nanomultilayersis an important research aspect, and the multilayer systems have alreadybeen extended based on the technical route of amorphous crystallizationoriginated from template effect, however, the nanomultilayers are mostlynitride based, rarely involving with carbides, bordides or oxides.
In order to extend the material systems from nitride to carbide basednanomultilayer, several TiC based nanomultilayers were designed on thebasis of TiC film preparation techniques, and these nanomultilayers areTiC/TiN multilayers composed of TiC and cubic nitride, TiC/WCmultilayers consisted by TiC and hybrid-structure carbide, TiC/Si_3N_4andTiC/SiC multilayers made of TiC and amorphous nitride, carbide,TiC/B_4C multilayers made up with TiC and B_4C which can react witheach other. The microstructure along with mechanical properties has beenstudied for the template effect of TiC with different types of materials andstructures， and the impact of modulation structure on mechanicalproperties of the multilayers has also been further studied. The research results not only reflect the extension of multilayer system, also promotethe understanding of the regulations between multilayer structure andsuperhardness effect.
1. For the TiC films prepared by reactive sputtering techniques,modulating the partial pressure of C_2H_2can control the film’scomposition, phase formation, microstructure as well as mechanicalproperties, and single phase, high hardness TiC films with bettercrystalline quality can be obtained in certain partial pressure, the highesthardness is31.6GPa. When TiC films are sputtered by compound target,the sputtering pressure (Ar) and substrate temperature can both influencecontent composition, deposition rate as well as film’s microstructure andmechanical properties, and the sputtering pressure has more obviouseffect on TiC films over substrate temperature.
Modulating the composition of TiC targets is an effective measure forobtaining single phase TiC films with better crystalline quality: TiC filmsprepared by stoichiometric TiC target, of which the content is located inTiC+C two phase region in phase diagram, may get poor crystallinity andmechanical properties owing to free carbon; TiC films, which wereprepared by substoichiometric TiC target with higher Ti content, wouldform double phase structure owing to high Ti content in TiC targets; TiCfilms, which were prepared by substoichiometric TiC target with a bit of overdosed Ti content，could obtain single phase TiC with higher hardnessand crystalline quality. By avoiding the reaction with other components inreactive atmosphere, preparing TiC films by substoichiometric TiC targetwith a bit of overdosed Ti is beneficial to match other components toform nanomultilayers.
2. The research of TiC_(0.8)/TiN and TiC_(1.0)/TiN nanomultilayers preparedby TiC targets using stoichiometric TiC target, substoichiometric TiCtarget with a bit of overdosed Ti content and TiN targets shows, theepitaxial growth structure formed in TiC_(0.8)/TiN nanomultilayers can beretained to the modulation period of14.4nm, and the multilayer can gainsuperhardness effect with highest hardness of38.6GPa. Athough theepitaxial growth structure formed in TiC_(1.0)/TiN nanomultilayers can beretained to the modulation period of3nm, the highest hardness inTiC_(1.0)/TiN nanomultilayers is only30.9GPa.
3. The investigation of TiC/WC nanomultilayers consisted of TiC andhybrid-structure WC shows that TiC layer can generate template effectthat can confine WC layer transiting to cubic structure, and undertemplate effect, WC layers can growth coherently with TiC layer in thesame structure when WC layer thickness is less than1.2nm. Meanwhile,crystal perfection is promoted by the mutual effect in the multilayer, andthe multilayer achieved its highest hardness of41.5GPa at0.5nm WC layer thickness. Further increasing the layer thickness, WC layers willturn back to the growth in multi-structure leading to the disruption ofcoherent growth structure and the decrease of hardness.
4. The investigation of TiC/Si_3N_4、TiC/SiC nanomultilayers consistedof TiC and amorphous Si_3N_4, SiC shows that, under the template effect ofTiC layers, amorphous Si_3N_4, SiC were forced to crystallized and growcoherently with TiC layers in the same structure when SiC and Si_3N_4layers is quite thin (about0.5nm), and the multilayers all appear hardnessincreased phenomenon with their highest of36.9GPa and37GPa,separately. Further increasing the layer thickness, the coherent growthstructure will be disrupted, and the hardness will decrease accordingly.
5. The research of TiC/B_4C nanomultilayers with interface reactionshows that when B_4C layer thickness is about0.5nm, the layer will allreact into TiB_2modulation layers, and the multilayer obtainsuperhardness effect with the highest hardness of40GPa. Furtherincreasing B_4C layer thickness, the non-reactive amorphous B_4C willdisrupt the coherent growth of the multilayers, the multilyers will formTiCx/TiB_2/B_4C triple layered structure, and the hardness will dropdramatically.Based on the research results, design requirements of thiskind of multilayers for achieving high hardness have been proposed:1.At least one modulation layer should be crystalline layer which is used as template layer for the new building layers;2. The other layer(amorphous layer included) should be as thin as possible (≤1nm) so thatthe interface reaction layers would all turn to the new building layers.3.The new building layers should be immiscible with the template layers;4. The template layers should have quiet large solid solubility to absorbthe excessive atoms generated in the reaction.
6. A series of nanomultilayers with different TiC and TiN layerthickness were used to reveal the impact regulation of modulationparameters on multilayers’ microstructure and mechanical properties.The results show that the multilayer can achieve high hardness onlywhen the multilayers can form sharp interface coherent growth structurewith modulation period and modulation layer thickness is quiet small;When modulation structure parameters change, decreasing themodulation layer thickness will lead to the increase of mixing layerthickness, increasing the layer thickness will lose the the amount ofinterface, especially when the coherent growth structure was disrupted,the hardness of the nanomultilayer will drop down quickly. The relationdiagram between modulation structure parameters and hardnessestablished in this paper can provide reference for designingnanomultilayers with superhardness effect.
Based on the research results above, new systems with superhardness effect have been obtained in TiC based nanomultilayers; The effect ofcrystallinity state in nanomultilayers has been revealed on the relationshipbetween microstructure and superhardness effect; The requirements fordesigning interface reactive nanomultilayers with superhardness effecthave been proposed; The design map of multilayer modulation structurehas been established.
为将高硬度纳米多层膜的材料体系由氮化物基拓展至碳化物基。论文在研究TiC薄膜制备技术的基础上，设计并制备了TiC与立方结构氮化物组成TiC/TiN纳米多层膜、混合结构碳化物组成TiC/WC纳米多层膜、非晶氮化物、碳化物组成TiC/Si_3N_4和TiC/SiC纳米多层膜、以及可反应碳化物组成TiC/B_4C纳米多层膜。研究了这些不同类型纳米多层膜的微结构和力学性能，并进一步揭示了纳米多层膜调制结构对其力学性能影响规律。
论文的主要结论如下：
1、采用反应溅射制备TiC薄膜时，通过调节C_2H_2分压可以控制TiC薄膜的成分、相组成、微结构和力学性能，合适的C_2H_2分压下可获得结晶好、硬度高的单相TiC薄膜，实验获得TiC薄膜最高硬度为31.6GPa。采用化合物靶溅射制备TiC时，薄膜的沉积速率、微结构、化学成分及力学性能皆受基片温度和溅射气压（Ar）的影响。其中溅射气压的影响较为明显，而基片温度在150℃-450℃间时对TiC薄膜结晶性能和硬度的影响有限。
陶瓷靶溅射制备TiC薄膜中，在TiC靶中增加Ti含量形成的富Ti靶(Ti:C=11:9)可获得结晶良好的单相TiC薄膜；化学计量比的TiC靶由于其成分处于相图TiC+C两相区，游离的C原子降低了薄膜的结晶程度和力学性能；而高富Ti的TiC靶（Ti:C=2:1）所得薄膜因产生Ti相而形成Ti+TiC两相结构。由于可避免反应溅射中反应气体与其他组成物的反应，采用富Ti的TiC靶(Ti:C=11:9)的直接溅射法更有益于与其他材料匹配制备纳米多层膜。
2、对由TiN分别与富钛和化学计量比的TiC靶制备的同晶体结构TiC_(0.8)/TiN和TiC_(1.0)/TiN纳米多层膜的研究发现，TiC_(0.8)/TiN纳米多层膜形成的共格外延生长结构可保持至14.4nm的调制周期，并获得最高硬度为38.6GPa的超硬效应。而TiC_(1.0)/TiN纳米多层膜虽也可在3.0nm的调制周期下获得共格外延生长结构，并获得超硬效应，但其最高硬度仅为30.9GPa。这一对比性结果揭示了组成物调制层的结晶状态对纳米多层膜的共格结构和超硬效应的重要影响。
3、对TiC与混合结构WC组成的TiC/WC纳米多层膜的研究表明，在TiC调制层的模板作用下，且WC层厚度小于约1.2nm时，多层膜将形成共格外延生长结构，此时WC层形成与TiC完全相同的立方结构调制层，多层膜的晶体完整性也因互促效应而得到显著提高，并在lWC=0.5nm时获得41.5GPa的最高硬度。当WC层因厚度的进一步增加时，其又转变为以混合结构形式生长，因而破坏了多层膜的共格外延结构，与其对应的多层膜硬度也随之降低。
4、在TiC与非晶态的Si_3N_4和SiC组成TiC/Si_3N_4、TiC/SiC的纳米多层膜中，由于TiC模板层作用，非晶态的SiC和Si_3N_4层均在厚度较薄时（约0.5nm）被晶化为与TiC相同的立方结构并与TiC层共格外延生长，两类多层膜都取得了硬度增高的超硬效应（其最高硬度分别为36.9GPa和37.0GPa）。随着SiC层和Si_3N_4层厚度的增加，多层膜的共格结构逐渐遭到破坏，硬度也逐渐降低。
5、对具有界面反应的TiC/B_4C纳米多层膜的研究发现，B_4C层在厚度约为0.5nm时全部反应生成TiB_2的调制层，多层膜转变为具有共格生长的TiCx/TiB_2纳米多层膜，并获得硬度异常增高的超硬效应，最高硬度达到40GPa。当B_4C调制层厚度进一步增加时，多层膜的共格外延生长结构因存在剩余未参与反应的非晶B_4C调制层而被破坏，多层膜形成TiCx/TiB_2/B_4C的三层结构，其硬度则相应显著降低。并基于实验结果提出了两调制层具有界面反应特征纳米多层膜获得超硬效应的设计要点：1、组成纳米多层膜的两调制层中至少一层需为晶体层，以作为界面反应层晶体生长的模板层；2、另一调制层（可为非晶层）的厚度应较小（≤1nm），以使其能够通过界面反应全部形成新的调制层；3、界面反应生成物与晶体模板层间应不具互溶性，以获得明锐的层间界面；4、较厚的晶体模板层应具有较大的固溶度，以能够吸收反应生成物中多余的游离原子。
6、对TiC/TiN纳米多层膜调制结构参数与力学性能关系的研究表明，只有当纳米多层膜的调制周期和各调制层的厚度均较小，调制层形成了清晰界面的层状结构并具有共格外延生长的结构特征时，多层膜才能产生硬度异常升高的超硬效应；而随调制结构参数的改变，减少调制层厚度将导致多层膜的界面混合区比例增大,增大调制层厚度则使界面数量减少，共格外延生长结构也会遭到破坏，这些结构的改变都使纳米多层膜的硬度明显降低。本文所建立的纳米多层膜调制结构参数与硬度的关系图可为纳米多层膜获得超硬效应的设计提供参考和借鉴。
基于以上研究结果，论文获得了一批具有超硬效应TiC基纳米多层膜的新体系；揭示了调制层结晶状态对纳米多层膜结构和超硬效应的影响规律；提出了具有界面反应的纳米多层膜体系材料和结构设计的要点；提出了纳米多层膜调制结构设计图。
The superhardness effect and diverse material combinations endowthe nanomultilayers with both high hardness and splendidcomprehensive properties. Widening the system of hard nanomultilayersis an important research aspect, and the multilayer systems have alreadybeen extended based on the technical route of amorphous crystallizationoriginated from template effect, however, the nanomultilayers are mostlynitride based, rarely involving with carbides, bordides or oxides.
In order to extend the material systems from nitride to carbide basednanomultilayer, several TiC based nanomultilayers were designed on thebasis of TiC film preparation techniques, and these nanomultilayers areTiC/TiN multilayers composed of TiC and cubic nitride, TiC/WCmultilayers consisted by TiC and hybrid-structure carbide, TiC/Si_3N_4andTiC/SiC multilayers made of TiC and amorphous nitride, carbide,TiC/B_4C multilayers made up with TiC and B_4C which can react witheach other. The microstructure along with mechanical properties has beenstudied for the template effect of TiC with different types of materials andstructures， and the impact of modulation structure on mechanicalproperties of the multilayers has also been further studied. The research results not only reflect the extension of multilayer system, also promotethe understanding of the regulations between multilayer structure andsuperhardness effect.
1. For the TiC films prepared by reactive sputtering techniques,modulating the partial pressure of C_2H_2can control the film’scomposition, phase formation, microstructure as well as mechanicalproperties, and single phase, high hardness TiC films with bettercrystalline quality can be obtained in certain partial pressure, the highesthardness is31.6GPa. When TiC films are sputtered by compound target,the sputtering pressure (Ar) and substrate temperature can both influencecontent composition, deposition rate as well as film’s microstructure andmechanical properties, and the sputtering pressure has more obviouseffect on TiC films over substrate temperature.
Modulating the composition of TiC targets is an effective measure forobtaining single phase TiC films with better crystalline quality: TiC filmsprepared by stoichiometric TiC target, of which the content is located inTiC+C two phase region in phase diagram, may get poor crystallinity andmechanical properties owing to free carbon; TiC films, which wereprepared by substoichiometric TiC target with higher Ti content, wouldform double phase structure owing to high Ti content in TiC targets; TiCfilms, which were prepared by substoichiometric TiC target with a bit of overdosed Ti content，could obtain single phase TiC with higher hardnessand crystalline quality. By avoiding the reaction with other components inreactive atmosphere, preparing TiC films by substoichiometric TiC targetwith a bit of overdosed Ti is beneficial to match other components toform nanomultilayers.
2. The research of TiC_(0.8)/TiN and TiC_(1.0)/TiN nanomultilayers preparedby TiC targets using stoichiometric TiC target, substoichiometric TiCtarget with a bit of overdosed Ti content and TiN targets shows, theepitaxial growth structure formed in TiC_(0.8)/TiN nanomultilayers can beretained to the modulation period of14.4nm, and the multilayer can gainsuperhardness effect with highest hardness of38.6GPa. Athough theepitaxial growth structure formed in TiC_(1.0)/TiN nanomultilayers can beretained to the modulation period of3nm, the highest hardness inTiC_(1.0)/TiN nanomultilayers is only30.9GPa.
3. The investigation of TiC/WC nanomultilayers consisted of TiC andhybrid-structure WC shows that TiC layer can generate template effectthat can confine WC layer transiting to cubic structure, and undertemplate effect, WC layers can growth coherently with TiC layer in thesame structure when WC layer thickness is less than1.2nm. Meanwhile,crystal perfection is promoted by the mutual effect in the multilayer, andthe multilayer achieved its highest hardness of41.5GPa at0.5nm WC layer thickness. Further increasing the layer thickness, WC layers willturn back to the growth in multi-structure leading to the disruption ofcoherent growth structure and the decrease of hardness.
4. The investigation of TiC/Si_3N_4、TiC/SiC nanomultilayers consistedof TiC and amorphous Si_3N_4, SiC shows that, under the template effect ofTiC layers, amorphous Si_3N_4, SiC were forced to crystallized and growcoherently with TiC layers in the same structure when SiC and Si_3N_4layers is quite thin (about0.5nm), and the multilayers all appear hardnessincreased phenomenon with their highest of36.9GPa and37GPa,separately. Further increasing the layer thickness, the coherent growthstructure will be disrupted, and the hardness will decrease accordingly.
5. The research of TiC/B_4C nanomultilayers with interface reactionshows that when B_4C layer thickness is about0.5nm, the layer will allreact into TiB_2modulation layers, and the multilayer obtainsuperhardness effect with the highest hardness of40GPa. Furtherincreasing B_4C layer thickness, the non-reactive amorphous B_4C willdisrupt the coherent growth of the multilayers, the multilyers will formTiCx/TiB_2/B_4C triple layered structure, and the hardness will dropdramatically.Based on the research results, design requirements of thiskind of multilayers for achieving high hardness have been proposed:1.At least one modulation layer should be crystalline layer which is used as template layer for the new building layers;2. The other layer(amorphous layer included) should be as thin as possible (≤1nm) so thatthe interface reaction layers would all turn to the new building layers.3.The new building layers should be immiscible with the template layers;4. The template layers should have quiet large solid solubility to absorbthe excessive atoms generated in the reaction.
6. A series of nanomultilayers with different TiC and TiN layerthickness were used to reveal the impact regulation of modulationparameters on multilayers’ microstructure and mechanical properties.The results show that the multilayer can achieve high hardness onlywhen the multilayers can form sharp interface coherent growth structurewith modulation period and modulation layer thickness is quiet small;When modulation structure parameters change, decreasing themodulation layer thickness will lead to the increase of mixing layerthickness, increasing the layer thickness will lose the the amount ofinterface, especially when the coherent growth structure was disrupted,the hardness of the nanomultilayer will drop down quickly. The relationdiagram between modulation structure parameters and hardnessestablished in this paper can provide reference for designingnanomultilayers with superhardness effect.
Based on the research results above, new systems with superhardness effect have been obtained in TiC based nanomultilayers; The effect ofcrystallinity state in nanomultilayers has been revealed on the relationshipbetween microstructure and superhardness effect; The requirements fordesigning interface reactive nanomultilayers with superhardness effecthave been proposed; The design map of multilayer modulation structurehas been established.
引文
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