The current study is directed to the rapidly developing field of inorganic material 3D object production at nano-/micro scale.The fabrication method includes laser lithography of hybrid organic-inorganic materials wit...The current study is directed to the rapidly developing field of inorganic material 3D object production at nano-/micro scale.The fabrication method includes laser lithography of hybrid organic-inorganic materials with subsequent heat treatment leading to a variety of crystalline phases in 3D structures.In this work,it was examined a series of organometallic polymer precursors with different silicon(Si)and zirconium(Zr)molar ratios,ranging from 9:1 to 5:5,prepared via sol-gel method.All mixtures were examined for perspective to be used in 3D laser manufacturing by fabricating nano-and micro-feature sized structures.Their spatial downscaling and surface morphology were evaluated depending on chemical composition and crystallographic phase.The appearance of a crystalline phase was proven using single-crystal X-ray diffraction analysis,which revealed a lower crystallization temperature for microstructures compared to bulk materials.Fabricated 3D objects retained a complex geometry without any distortion after heat treatment up to 1400℃.Under the proper conditions,a wide variety of crystalline phases as well as zircon(ZrSiO_(4)-a highly stable material)can be observed.In addition,the highest new record of achieved resolution below 60 nm has been reached.The proposed preparation protocol can be used to manufacture micro/nano-devices with high precision and resistance to high temperature and aggressive environment.展开更多
Here we report a femtosecond laser direct writing(a precise 3D printing also known as two-photon polymerization lithography) of hybrid organic-inorganic SZ2080^(TM)pre-polymer without using any photo-initiator and app...Here we report a femtosecond laser direct writing(a precise 3D printing also known as two-photon polymerization lithography) of hybrid organic-inorganic SZ2080^(TM)pre-polymer without using any photo-initiator and applying ~100 fs oscillator operating at 517 nm wavelength and 76 MHz repetition rate. The proof of concept was experimentally demonstrated and benchmarking 3D woodpile nanostructures, micro-scaffolds, free-form micro-object “Benchy” and bulk micro-cubes are successfully produced. The essential novelty underlies the fact that non-amplified laser systems delivering just 40-500 p J individual pulses are sufficient for inducing localized cross-linking reactions within hundreds of nanometers in cross sections. And it is opposed to the prejudice that higher pulse energies and lower repetition rates of amplified lasers are necessary for structuring non-photosensitized polymers. The experimental work is of high importance for fundamental understanding of laser enabled nanoscale 3D additive manufacturing and widens technology’ s field of applications where the avoidance of photo-initiator is preferable or is even a necessity, such as micro-optics, nano-photonics, and biomedicine.展开更多
The shear failure of intact rock under thermo-mechanical(TM)coupling conditions is common,such as in enhanced geothermal mining and deep mine construction.Under the effect of a continuous engineering disturbance,shear...The shear failure of intact rock under thermo-mechanical(TM)coupling conditions is common,such as in enhanced geothermal mining and deep mine construction.Under the effect of a continuous engineering disturbance,shear-formed fractures are prone to secondary instability,posing a severe threat to deep engineering.Although numerous studies regarding three-dimensional(3D)morphologies of fracture surfaces have been conducted,the understanding of shear-formed fractures under TM coupling conditions is limited.In this study,direct shear tests of intact granite under various TM coupling conditions were conducted,followed by 3D laser scanning tests of shear-formed fractures.Test results demonstrated that the peak shear strength of intact granite is positively correlated with the normal stress,whereas it is negatively correlated with the temperature.The internal friction angle and cohesion of intact granite significantly decrease with an increase in the temperature.The anisotropy,roughness value,and height of the asperities on the fracture surfaces are reduced as the normal stress increases,whereas their variation trends are the opposite as the temperature increases.The macroscopic failure mode of intact granite under TM coupling conditions is dominated by mixed tensileeshear and shear failures.As the normal stress increases,intragranular fractures are developed ranging from a local to a global distribution,and the macroscopic failure mode of intact granite changes from mixed tensileeshear to shear failure.Finally,3D morphological characteristics of the asperities on the shear-formed fracture surfaces were analyzed,and a quadrangular pyramid conceptual model representing these asperities was proposed and sufficiently verified.展开更多
基金The US AMRDEC grant No.W911NF-16-2-0069“Enhanced Absorption in Stopped-Light Photonic Nanostructures:Applications to Efficient Sensing”EU LASERLAB-EUROPE(grant agreement No.871124Horizon 2020 research and innovation programme)projects are acknowleged for the financial support.D.G.acknowledges the financial support from the European Social Fund(project No 09.3.3-LMT-K712-17-0016)under grant agreement with the Research Council of Lithuania(LMTLT).
文摘The current study is directed to the rapidly developing field of inorganic material 3D object production at nano-/micro scale.The fabrication method includes laser lithography of hybrid organic-inorganic materials with subsequent heat treatment leading to a variety of crystalline phases in 3D structures.In this work,it was examined a series of organometallic polymer precursors with different silicon(Si)and zirconium(Zr)molar ratios,ranging from 9:1 to 5:5,prepared via sol-gel method.All mixtures were examined for perspective to be used in 3D laser manufacturing by fabricating nano-and micro-feature sized structures.Their spatial downscaling and surface morphology were evaluated depending on chemical composition and crystallographic phase.The appearance of a crystalline phase was proven using single-crystal X-ray diffraction analysis,which revealed a lower crystallization temperature for microstructures compared to bulk materials.Fabricated 3D objects retained a complex geometry without any distortion after heat treatment up to 1400℃.Under the proper conditions,a wide variety of crystalline phases as well as zircon(ZrSiO_(4)-a highly stable material)can be observed.In addition,the highest new record of achieved resolution below 60 nm has been reached.The proposed preparation protocol can be used to manufacture micro/nano-devices with high precision and resistance to high temperature and aggressive environment.
基金Project(S-MIP-20-17) supported by the Research Council of LithuaniaProject(871124) supported by the EU Horizon 2020, Research and Innovation program LASERLAB-EUROPE JRA。
文摘Here we report a femtosecond laser direct writing(a precise 3D printing also known as two-photon polymerization lithography) of hybrid organic-inorganic SZ2080^(TM)pre-polymer without using any photo-initiator and applying ~100 fs oscillator operating at 517 nm wavelength and 76 MHz repetition rate. The proof of concept was experimentally demonstrated and benchmarking 3D woodpile nanostructures, micro-scaffolds, free-form micro-object “Benchy” and bulk micro-cubes are successfully produced. The essential novelty underlies the fact that non-amplified laser systems delivering just 40-500 p J individual pulses are sufficient for inducing localized cross-linking reactions within hundreds of nanometers in cross sections. And it is opposed to the prejudice that higher pulse energies and lower repetition rates of amplified lasers are necessary for structuring non-photosensitized polymers. The experimental work is of high importance for fundamental understanding of laser enabled nanoscale 3D additive manufacturing and widens technology’ s field of applications where the avoidance of photo-initiator is preferable or is even a necessity, such as micro-optics, nano-photonics, and biomedicine.
基金supported by the National Natural Science Foundation of China(Grant No.51974173)the Natural Science Foundation of Shandong Province,China(Grant No.ZR2020QD122).
文摘The shear failure of intact rock under thermo-mechanical(TM)coupling conditions is common,such as in enhanced geothermal mining and deep mine construction.Under the effect of a continuous engineering disturbance,shear-formed fractures are prone to secondary instability,posing a severe threat to deep engineering.Although numerous studies regarding three-dimensional(3D)morphologies of fracture surfaces have been conducted,the understanding of shear-formed fractures under TM coupling conditions is limited.In this study,direct shear tests of intact granite under various TM coupling conditions were conducted,followed by 3D laser scanning tests of shear-formed fractures.Test results demonstrated that the peak shear strength of intact granite is positively correlated with the normal stress,whereas it is negatively correlated with the temperature.The internal friction angle and cohesion of intact granite significantly decrease with an increase in the temperature.The anisotropy,roughness value,and height of the asperities on the fracture surfaces are reduced as the normal stress increases,whereas their variation trends are the opposite as the temperature increases.The macroscopic failure mode of intact granite under TM coupling conditions is dominated by mixed tensileeshear and shear failures.As the normal stress increases,intragranular fractures are developed ranging from a local to a global distribution,and the macroscopic failure mode of intact granite changes from mixed tensileeshear to shear failure.Finally,3D morphological characteristics of the asperities on the shear-formed fracture surfaces were analyzed,and a quadrangular pyramid conceptual model representing these asperities was proposed and sufficiently verified.
