Structural properties of residual carbon in coal gasification fine slag and their influence on flotation separation and resource utilization:A review

Coal gasification fine slag(FS)is a typical solid waste generated in coal gasification.Its current disposal methods of stockpil-ing and landfilling have caused serious soil and ecological hazards.Separation recovery and the high-value utilization of residual carbon(RC)in FS are the keys to realizing the win-win situation of the coal chemical industry in terms of economic and environmental benefits.The structural properties,such as pore,surface functional group,and microcrystalline structures,of RC in FS(FS-RC)not only affect the flotation recovery efficiency of FS-RC but also form the basis for the high-value utilization of FS-RC.In this paper,the characteristics of FS-RC in terms of pore structure,surface functional groups,and microcrystalline structure are sorted out in accordance with gasification type and FS particle size.The reasons for the formation of the special structural properties of FS-RC are analyzed,and their influence on the flotation separation and high-value utilization of FS-RC is summarized.Separation methods based on the pore structural characterist-ics of FS-RC,such as ultrasonic pretreatment-pore-blocking flotation and pore breaking-flocculation flotation,are proposed to be the key development technologies for improving FS-RC recovery in the future.The design of low-cost,low-dose collectors containing polar bonds based on the surface and microcrystalline structures of FS-RC is proposed to be an important breakthrough point for strengthening the flotation efficiency of FS-RC in the future.The high-value utilization of FS should be based on the physicochemical structural proper-ties of FS-RC and should focus on the environmental impact of hazardous elements and the recyclability of chemical waste liquid to es-tablish an environmentally friendly utilization method.This review is of great theoretical importance for the comprehensive understand-ing of the unique structural properties of FS-RC,the breakthrough of the technological bottleneck in the efficient flotation separation of FS,and the expansion of the field of the high value-added utilization of FS-RC.

Harness High-Temperature Thermal Energy via Elastic Thermoelectric Aerogels

Despite notable progress in thermoelectric(TE)materials and devices,developing TE aerogels with high-temperature resistance,superior TE performance and excellent elasticity to enable self-powered high-temperature monitoring/warning in industrial and wearable applications remains a great challenge.Herein,a highly elastic,flame-retardant and high-temperature-resistant TE aerogel,made of poly(3,4-ethylene dioxythiophene):poly(styrenesulfonate)/single-walled carbon nanotube(PEDOT:PSS/SWCNT)composites,has been fabricated,displaying attractive compression-induced power factor enhancement.The as-fabricated sensors with the aerogel can achieve accurately pressure stimuli detection and wide temperature range monitoring.Subsequently,a flexible TE generator is assembled,consisting of 25 aerogels connected in series,capable of delivering a maximum output power of 400μW when subjected to a temperature difference of 300 K.This demonstrates its outstanding high-temperature heat harvesting capability and promising application prospects for real-time temperature monitoring on industrial high-temperature pipelines.Moreover,the designed self-powered wearable sensing glove can realize precise wide-range temperature detection,high-temperature warning and accurate recognition of human hand gestures.The aerogel-based intelligent wearable sensing system developed for firefighters demonstrates the desired self-powered and highly sensitive high-temperature fire warning capability.Benefitting from these desirable properties,the elastic and high-temperature-resistant aerogels present various promising applications including self-powered high-temperature monitoring,industrial overheat warning,waste heat energy recycling and even wearable healthcare.

Synergistic effect of Zr and Mo on precipitation and high-temperature properties of Al-Si-Cu-Mg alloys

This study focuses on finding a solution to the sharp decline in mechanical properties of Al-Si-Cu-Mg alloys due to rapid coarsening of traditional intermediate phases at high temperature.A new type of modified al oy,to be used in automobile engines at high temperatures,was prepared by adding Zr and Mo into Al-Si-Cu-Mg alloy.The synergistic effects of Zr and Mo on the microstructure evolution and high-temperature mechanical properties were studied.Results show that the addition of Zr and Mo generates a series of intermetallic phases dispersed in the alloy.They can improve the strength of the alloy by hindering dislocation movement and crack propagation.In addition,some nano-strengthened phases show coherent interfaces with the matrix and improve grain refinement.The addition of Mo greatly improves the heat resistance of the alloy.The extremely low diffusivity of Mo enables it to improve the thermal stability of the intermetallic phases,inhibit precipitation during aging,reduce the size of the precipitates,and improve the heat resistance of the alloy.

HZSM-5 zeolites undergoing the high-temperature process for boosting the bimolecular reaction in n-heptane catalytic cracking

High-temperature treatment is key to the preparation of zeolite catalysts.Herein,the effects of hightemperature treatment on the property and performance of HZSM-5 zeolites were studied in this work.X-Ray diffraction,N2physisorption,27Al magic angle spinning nuclear magnetic resonance(MAS NMR),and temperature-programmed desorption of ammonia results indicated that the hightemperature treatment at 650℃ hardly affected the inherent crystal and texture of HZSM-5zeolites but facilitated the conversion of framework Al to extra-framework Al,reducing the acid site and enhancing the acid strength.Moreover,the high-temperature treatment improved the performance of HZSM-5 zeolites in n-heptane catalytic cracking,promoting the conversion and light olefins yield while inhibiting coke formation.Based on the kinetic and mechanism analysis,the improvement of HZSM-5 performance caused by high-temperature treatment has been attributed to the formation of extra-framework Al,which enhanced the acid strength,facilitated the bimolecular reaction,and promoted the entropy change to overcome a higher energy barrier in n-heptane catalytic cracking.

Experimental study on the activation of coal gasification fly ash from industrial CFB gasifiers

Coal gasification fly ash(CGFA)is an industrial solid waste from the coal circulating fluidized bed(CFB)gasification process,and it needs to be effectively disposed to achieve sustainable development of the environment.To realize the application of CGFA as a precursor of porous carbon materials,the physicochemical properties of three kinds of CGFA from industrial CFB gasifiers are analyzed.Then,the activation potential of CGFA is acquired via steam activation experiments in a tube furnace reactor.Finally,the fluidization activation technology of CGFA is practiced in a bench-scale CFB test rig,and its advantages are highlighted.The results show that CGFA is characterized by a high carbon content in the range of 54.06%–74.09%,an ultrafine particle size(d50:16.3–26.1 μm),and a relatively developed pore structure(specific surface area SSA:139.29–551.97 m^(2)·g^(-1)).The proportion of micropores in CGFA increases gradually with the coal rank.Steam activation experiments show that the pore development of CGFA mainly includes three stages:initial pore development,dynamic equilibrium between micropores and mesopores and pore collapse.The SSA of lignite fly ash(LFA),subbituminous fly ash(SBFA)and anthracite fly ash(AFA)is maximally increased by 105%,13%and 72%after steam activation;the order of the largest carbon reaction rate and decomposition ratio of steam among the three kinds of CGFA is SBFA>LFA>AFA.As the ratio of oxygen to carbon during the fluidization activation of LFA is from 0.09 to 0.19,the carbon conversion ratio increases from 14.4%to 26.8%and the cold gas efficiency increases from 6.8%to 10.2%.The SSA of LFA increases by up to 53.9%during the fluidization activation process,which is mainly due to the mesoporous development.Relative to steam activation in a tube furnace reactor,fluidization activation takes an extremely short time(seconds)to achieve the same activation effect.It is expected to further improve the activation effect of LFA by regulating the carbon conversion ratio range of 27%–35%to create pores in the initial development stage.

Novel Method for Evaluating the Aging of Aviation Turbine Engine Oils via High-Temperature Bearing Deposit Tests

Aviation turbine engine oils require excellent thermal-oxidative stability because of their high-temperature environments.High-temperature bearing deposit testing is a mandatory method for measuring the thermal-oxidative performance of aviation lubricant oils,and the relevant apparatus was improved in the present study.Two different commercial aviation turbine engine oils were tested,one with standard performance(known as the SL oil)and the other with high thermal stability,and their thermal-oxidative stability characteristics were evaluated.After 100 h of high-temperature bearing testing,the SL oil was analyzed by using various analytical techniques to investigate its thermal-oxidative process in the bearing test,with its thermal-oxidative degradation mechanism also being discussed.The results indicate that the developed high-temperature bearing apparatus easily meets the test requirements of method 3410.1 in standard FED-STD-791D.The viscosity and total acid number(TAN)of the SL oil increased with the bearing test time,and various deposits were produced in the bearing test,with the micro-particles of the carbon deposits being sphere-like,rod-like,and sheet-like in appearance.The antioxidant additives in the oil were consumed very rapidly in the first 30 h of the bearing test,with N-phenyl-1-naphthylamine being consumed faster than dioctyldiphenylamine.Overall,the oil thermal-oxidative process involves very complex physical and chemical mechanisms.

High-performance and robust high-temperature polymer electrolyte membranes with moderate microphase separation by implementation of terphenyl-based polymers

Acid loss and plasticization of phosphoric acid(PA)-doped high-temperature polymer electrolyte membranes(HT-PEMs)are critical limitations to their practical application in fuel cells.To overcome these barriers,poly(terphenyl piperidinium)s constructed from the m-and p-isomers of terphenyl were synthesized to regulate the microstructure of the membrane.Highly rigid p-terphenyl units prompt the formation of moderate PA aggregates,where the ion-pair interaction between piperidinium and biphosphate is reinforced,leading to a reduction in the plasticizing effect.As a result,there are trade-offs between the proton conductivity,mechanical strength,and PA retention of the membranes with varied m/p-isomer ratios.The designed PA-doped PTP-20m membrane exhibits superior ionic conductivity,good mechanical strength,and excellent PA retention over a wide range of temperature(80–160°C)as well as satisfactory resistance to harsh accelerated aging tests.As a result,the membrane presents a desirable combination of performance(1.462 W cm^(-2) under the H_(2)/O_(2)condition,which is 1.5 times higher than that of PBI-based membrane)and durability(300 h at 160°C and 0.2 A cm^(-2))in the fuel cell.The results of this study provide new insights that will guide molecular design from the perspective of microstructure to improve the performance and robustness of HT-PEMs.

Integrated multi-scale approach combining global homogenization and local refinement for multi-field analysis of high-temperature superconducting composite magnets

Second-generation high-temperature superconducting(HTS)conductors,specifically rare earth-barium-copper-oxide(REBCO)coated conductor(CC)tapes,are promising candidates for high-energy and high-field superconducting applications.With respect to epoxy-impregnated REBCO composite magnets that comprise multilayer components,the thermomechanical characteristics of each component differ considerably under extremely low temperatures and strong electromagnetic fields.Traditional numerical models include homogenized orthotropic models,which simplify overall field calculation but miss detailed multi-physics aspects,and full refinement(FR)ones that are thorough but computationally demanding.Herein,we propose an extended multi-scale approach for analyzing the multi-field characteristics of an epoxy-impregnated composite magnet assembled by HTS pancake coils.This approach combines a global homogenization(GH)scheme based on the homogenized electromagnetic T-A model,a method for solving Maxwell's equations for superconducting materials based on the current vector potential T and the magnetic field vector potential A,and a homogenized orthotropic thermoelastic model to assess the electromagnetic and thermoelastic properties at the macroscopic scale.We then identify“dangerous regions”at the macroscopic scale and obtain finer details using a local refinement(LR)scheme to capture the responses of each component material in the HTS composite tapes at the mesoscopic scale.The results of the present GH-LR multi-scale approach agree well with those of the FR scheme and the experimental data in the literature,indicating that the present approach is accurate and efficient.The proposed GH-LR multi-scale approach can serve as a valuable tool for evaluating the risk of failure in large-scale HTS composite magnets.

Occurrence,leaching behavior,and detoxification of heavy metal Cr in coal gasification slag

Coal gasification slag(CGS)is a type of solid waste produced during coal gasification,in which heavy metals severely restrict its resource utilization.In this work,the mineral occurrence and distribution of typical heavy metal Cr in CGS is investigated.The leaching behavior of Cr under different conditions is studied in detail.Acid leaching-selective oxidation-coprecipitation method is proposed based on the characteristics of Cr in CGS.The detoxification of Cr in CGS is realized,and the detoxification mechanism is clarified.Results show that Cr is highly enriched in CGS.The speciation of Cr is mainly residual fraction(74.47%-86.12%),which is combined with amorphous aluminosilicate.Cr^(3+)and Cr^(6+)account for 90.93%-94.82%and 5.18%-9.07%of total Cr,respectively.High acid concentration and high liquid-solid ratio are beneficial to destroy the lattice structure of amorphous aluminosilicate,thus improving the leaching efficiency of Cr,which can reach 97.93%under the optimal conditions.Acid leaching-selective oxidation-coprecipitation method can realize the detoxification of Cr in CGS.Under the optimal conditions,the removal rates of Fe^(3+)and Cr^(3+)in the leaching solution are 80.99%-84.79%and 70.58%-71.69%,respectively,while the loss rate of Al^(3+)is only 1.10%-3.35%.Detoxification slag exists in the form of Fe-Cr coprecipitation(Fe_(1-x)Cr_xOOH),which can be used for smelting.The detoxification acid leaching solution can be used to prepare inorganic polymer composite coagulant poly-aluminum chloride(PAC).This study can provide theoretical and data guidance for detoxification of heavy metal Cr in CGS and achieve resource utilization of coal gasification solid waste.

Seasonal Prediction of Extreme High-Temperature Days in Southwestern China Based on the Physical Precursors

Extreme high temperatures frequently occur in southwestern China,significantly impacting the local ecological system and economic development.However,accurate prediction of extreme high-temperature days(EHDs)in this region is still an unresolved challenge.Based on the spatiotemporal characteristics of EHDs over China,a domain-averaged EHD index over southwestern China(SWC-EHDs)during April-May is defined.The simultaneous dynamic and thermodynamic fields associated with the increased SWC-EHDs are a local upper-level anticyclonic(high-pressure)anomaly and wavy geopotential height anomaly patterns over Eurasia.In tracing the origins of the lower boundary anomalies,two physically meaningful precursors are detected for SWC-EHDs.They are the tripolar SST change tendency from December-January to February-March in the northern Atlantic and the February-March mean snow depth in central Asia.Using these two selected predictors,a physics-based empirical model prediction was applied to the training period of 1961–2005 to obtain a skillful prediction of the EHDs index,attaining a correlation coefficient of 0.76 in the independent prediction period(2006–19),suggesting that 58%of the total SWC-EHDs variability is predictable.This study provides an estimate for the lower bound of the seasonal predictability of EHDs as well as for the hydrological drought over southwestern China.

Research on the impact of high-temperature aging on the thermal safety of lithium-ion batteries

Understanding the thermal safety evolution of lithium-ion batteries during high-temperature usage conditions bears significant implications for enhancing the safety management of aging batteries.This work investigates the thermal safety evolution mechanism of lithium-ion batteries during high-temperature aging.Similarities arise in the thermal safety evolution and degradation mechanisms for lithium-ion batteries undergoing cyclic aging and calendar aging.Employing multi-angle characterization analysis,the intricate mechanism governing the thermal safety evolution of lithium-ion batteries during high-temperature aging is clarified.Specifically,lithium plating serves as the pivotal factor contributing to the reduction in the self-heating initial temperature.Additionally,the crystal structure of the cathode induced by the dissolution of transition metals and the reductive gas generated during aging attacking the crystal structure of the cathode lead to a decrease in thermal runaway triggering temperature.Furthermore,the loss of active materials and active lithium during aging contributes to a decline in both the maximum temperature and the maximum temperature rise rate,ultimately indicating a decrease in the thermal hazards of aging batteries.

Study on the effect of thermal deformation on the liquid seal of high-temperature molten salt pump in molten salt reactor

The high-temperature molten salt pump is the core equipment in a molten salt reactor that drives the flow of the molten salt coolant.Rotor stability is key to the continuous and reliable operation of the molten salt pump,and the liquid seal at the wear ring can affect the dynamic characteristics of the rotor system.When the molten salt pump is operated in the hightemperature molten salt medium,thermal deformation of the submerged parts inevitably occurs,changing clearance between the stator and rotor,affecting the leakage and dynamic characteristics of the seal.In this study,the seal leakage,seal dynamic characteristics,and rotor system dynamic characteristics are simulated and analyzed using finite element simulation software based on two cases of considering the effect of seal thermal deformation effect or not.The results show a significant difference in the leakage characteristics and dynamic characteristics of the seal obtained by considering the effect of seal thermal deformation and neglecting the effect of thermal deformation.The leakage flow rate decreases,and the first-order critical speed of the seal-bearing-rotor system decrease after considering the seal’s thermal deformation.

Integrated vacuum pressure swing adsorption and Rectisol process for CO_(2) capture from underground coal gasification syngas

An integrated vacuum pressure swing adsorption(VPSA) and Rectisol process is proposed for CO_(2) capture from underground coal gasification(UCG) syngas. A ten-bed VPSA process with silica gel adsorbent is firstly designed to pre-separate and capture 74.57% CO_(2) with a CO_(2) purity of 98.35% from UCG syngas(CH_(4)/CO/CO_(2)/H_(2)/N_(2)= 30.77%/6.15%/44.10%/18.46%/0.52%, mole fraction, from Shaar Lake Mine Field,Xinjiang Province, China) with a feed pressure of 3.5 MPa. Subsequently, the Rectisol process is constructed to furtherly remove and capture the residual CO_(2)remained in light product gas from the VPSA process using cryogenic methanol(233.15 K, 100%(mass)) as absorbent. A final purified gas with CO_(2) concentration lower than 3% and a regenerated CO_(2) product with CO_(2) purity higher than 95% were achieved by using the Rectisol process. Comparisons indicate that the energy consumption is deceased from 2.143 MJ·kg^(-1) of the single Rectisol process to 1.008 MJ·kg^(-1) of the integrated VPSA & Rectisol process, which demonstrated that the deployed VPSA was an energy conservation process for CO_(2) capture from UCG syngas. Additionally, the high-value gas(e.g., CH_(4)) loss can be decreased and the effects of key operating parameters on the process performances were detailed.

High-temperature stress suppresses allene oxide cyclase 2 and causes male sterility in cotton by disrupting jasmonic acid signaling

Cotton(Gossypium spp.) yield is reduced by stress. In this study, high temperature(HT) suppressed the expression of the jasmonic acid(JA) biosynthesis gene allene oxide cyclase 2(GhAOC2), reducing JA content and causing male sterility in the cotton HT-sensitive line H05. Anther sterility was reversed by exogenous application of methyl jasmonate(MeJA) to early buds. To elucidate the role of GhAOC2 in JA biosynthesis and identify its putative contribution to the anther response to HT, we created gene knockout cotton plants using the CRISPR/Cas9 system. Ghaoc2 mutant lines showed male-sterile flowers with reduced JA content in the anthers at the tetrad stage(TS), tapetum degradation stage(TDS), and anther dehiscence stage(ADS). Exogenous application of MeJA to early mutant buds(containing TS or TDS anthers) rescued the sterile pollen and indehiscent anther phenotypes, while ROS signals were reduced in ADS anthers. We propose that HT downregulates the expression of GhAOC2 in anthers, reducing JA biosynthesis and causing excessive ROS accumulation in anthers, leading to male sterility. These findings suggest exogenous JA application as a strategy for increasing male fertility in cotton under HT.

Recycling and utilization of coal gasification residues for fabricating Fe/C composites as novel microwave absorbents

Under the background of a transformation of the global energy structure,coal gasification technology has a wide application prospect,but its by-product,the coal gasification residue(CGR),is still not being efficiently utilized for recycling.The CGR contains abundant carbon components,which could be applied to the microwave absorption field as the carbon matrix.In this study,Fe/CGR composites are fabricated via a two-step method,including the impregnation of Fe^(3+)and the reduction process.The influence of the different loading capacities of the Fe component on the morphology and electromagnetic properties is studied.Moreover,the loading content of Fe and the surface morphology of the Fe/CGR can be reasonably controlled by adjusting the concentration of the ferric nitrate solution.Meanwhile,Fe particles are evenly inserted on the CGR framework,which expands the Fe/CGR interfaces to enhance interfacial polarization,thus further improving the microwave-absorbing(MA)properties of composites.Particularly,as the Fe^(3+)concentration is 1.0 mol/L,the Fe/CGR composite exhibits outstanding performance.The reflection loss reaches-39.3 dB at 2.5 mm,and the absorption bandwidth covers 4.1 GHz at 1.5 mm.In this study,facile processability,resource recycling,appropriately matched impedance,and excellent MA performance are achieved.Finally,the Fe/CGR composites not only enhance the recycling of the CGR but also pioneer a new path for the synthesis of excellent absorbents.

Effects of Different Calcining Temperatures on the Properties of Ceramsite Prepared by High-carbon Gasification Slag

The structure and characteristics of high-performance lightweight aggregates produced by high-carbon gasification slag were investigated by X-ray diffraction,scanning electron microscopy,thermogravimetry/differential thermogravimetr,differential scanning calorimetry-Fourier transform infrared,and mercury intrusion porosimetry,respectively.The experimental results show that the ceramsite undergoes two weightless stages in the calcining process.With the increase in the calcining temperature,a large number of pores are formed inside the ceramsite,its structure becomes denser,but the calcining temperature band of the ceramsite becomes narrow.The crystalline phase of the ceramsite changes at different calcining temperatures and the mineral phase changes from the earlieralbite,quartz,oligoclase,hematite,etc,to a silica-aluminum-rich glass phase.The 1130℃ is a more suitable calcining temperature,and the cylinder compressive strength of ceramics is 11.59 MPa,the packing density,apparent density,porosity,and water absorption are 939.11 kg/m^(3),1643.75 kg/m^(3),28.11%,and 10.35%,respectively,which can meet the standards for high-strength lightweight aggregates.

Gasification kinetic studies of low volatile weakly caking coal

Present investigation focuses on the fractional conversion of low volatile weakly caking coal(LVWC)under the standard set of operating conditions for gasification.For this purpose,samples of LVWC of different ash content have been collected from Kusunda Area of Bharat Coking Coal Ltd.Gasification results were validated using Homogenous and Shrinking Core kinetic models and the suitability of selected samples for gasification was assessed by estimating the activation energy.The values of activation energy for LVWC samples were obtained in the range of 25.17-44.09 kJ/mol.Further,empirical models were developed to correlate the response of interest with the input variables(temperature,residence time and CO_(2) flow rate).The significance of these developed empirical models was checked using analysis of variance(ANOVA).

A 3–5μm broadband YBCO high-temperature superconducting photonic crystal

Photonic crystal structures have excellent optical properties,so they are widely studied in conventional optical materials.Recent research shows that high-temperature superconducting periodic structures have natural photonic crystal features and they are favourable candidates for single-photon detection.Considering that superconductors have completely different properties from conventional optical materials,we study the energy level diagram and mid-infrared 3μm–5μm transmission spectrum of two-dimensional superconducting photonic crystals in both superconducting and quenched states with the finite element method.The energy level diagram of the circular crystal column superconducting structure shows that the structure has a large band gap width in both states.At the same fill factor,the circular crystal column superconducting structure has a larger band gap width than the others structures.For lattice structures,the zero transmission point of the square lattice structure is robust to the incident angle and environmental temperature.Our research has guiding significance for the design of new material photonic crystals,photon modulation and detection.

Gasification of Organic Waste:Parameters,Mechanism and Prediction with the Machine Learning Approach

Gasification of organic waste represents one of the most effective valorization pathways for renewable energy and resources recovery,while this process can be affected by multi-factors like temperature,feedstock,and steam content,making the product’s prediction problematic.With the popularization and promotion of artificial intelligence such as machine learning(ML),traditional artificial neural networks have been paid more attention by researchers from the data science field,which provides scientific and engineering communities with flexible and rapid prediction frameworks in the field of organic waste gasification.In this work,critical parameters including temperature,steam ratio,and feedstock during gasification of organic waste were reviewed in three scenarios including steam gasification,air gasification,and oxygen-riched gasification,and the product distribution and involved mechanism were elaborated.Moreover,we presented the details of ML methods like regression analysis,artificial neural networks,decision trees,and related methods,which are expected to revolutionize data analysis and modeling of the gasification of organic waste.Typical outputs including the syngas yield,composition,and HHVs were discussed with a better understanding of the gasification process and ML application.This review focused on the combination of gasification and ML,and it is of immediate significance for the resource and energy utilization of organic waste.

Enhancement of the Mechanical Performance of SiCf/Phenolic Composites after High-temperature Pyrolysis Using ZrC/B_(4)C Particles

The composites were prepared by modifying silicon carbide fiber with particles of zirconium carbide(ZrC)and boron carbide(B_(4)C)and incorporating them into a phenolic resin matrix.The influence of ZrC and B_(4)C on the mechanical performance of SiCf/phenolic composites after high-temperature pyrolysis was studied through flexural performance test.The results show that the composite material has good thermal stability and high-temperature mechanical properties.After static ablation at 1400℃ for 15 minutes,the flexural strength of the composite material reaches 286 MPa,which is still 7.3%higher than at room temperature,indicating that the composite material still has good mechanical properties even after heat treatment at 1400℃.