DIFFERENTIAL SCANNING CALORIMETRY AND X-RAY DIFFRACTION STUDIES ON AGING BEHAVIOR OF Zn-Al ALLOYS

Decomposition processes of the quenched Zn-Al alloys were studied by differential scanning calorimetry (DSC), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the stabilities of supersaturated solid solution (SSS) of Zn-Al alloy and α' phase formed by quenching would reduce with the increase of Zn content and the precipitation of η-Zn phases even when aging at ambient temperature, so that the exothermic precipitation peak in DSC curve would disappear. The activation energy of the η-Zn precipitation and the reaction enthalpy were calculated and measured. The kinetics of α' decomposition or η-Zn formation was determined by XRD. The microstructure change during aging was observed by TEM.

Assessment of parameters for precipitation simulation of heat treatable aluminum alloys using differential scanning calorimetry

Differential scanning calorimetry （DSC） has been used extensively to study different solid state reactions. The signals measured in DSC are associated with the growth and dissolution of different precipitates during a specific heat cycle. The time-temperature dependence of heat cycles and the corresponding heat flow evolution measured in the sample by DSC provide valuable experimental information about the phase evolution and the precipitation kinetics in the material. The thermo-kinetic computer simulation was used to predict the DSC signals of samples taken from 6xxx and 2xxx alloys. In the model, the evolution of different metastable and stable phases and the role and influence of excess quenched-in vacancies in the early stage of precipitation were taken into account. Transmission electron microscopy （TEM） and high-resolution TEM were used to verify the existence of precipitates, their size and number density at specific points of the DSC curves.

Research on thermal decomposition of 1,3,5-trinitro-1,3,5-triazinane based on differential scanning calorimetry

In order to test the thermal decomposition of 1,3,5-trinitro-1,3,5-triazinane(RDX),the linear temperature rise experiment of RDX was carried out by differential scanning calorimeter under different heating rate conditions.The kinetic calculation of RDX thermal decomposition curve was carried out by Kissinger and Ozawa methods,respectively,and the thermal analysis software was used to calculate the parameters such as self-accelerating decomposition temperature.The results show that the initial decomposition temperature range,decomposition peak temperature range,and decomposition completion temperature range of RDX are 208.4-214.2,225.7-239.3 and 234.0-252.4℃,respectively,and the average decomposition enthalpy is 362.9 J·g^-1.Kissinger method was used to calculate the DSC experimental data of RDX,the apparent activation energy obtained is 190.8 kJ·mol^-1,which is coincident with the results calculated by Ozawa method at the end of the reaction,indicating that the apparent activation energy calculated by the two methods is relatively accurate.When the packaging mass values are 1.0,2.0 and 5.0 kg,respectively,the self-accelerating decomposition temperatures are 97.0,93.0 and 87.0℃,respectively,indicating that with the increase of packaging mass,the self-accelerating decomposition temperature gradually decreases,and the risk increases accordingly.

Synthesis kinetics of Mg_2Sn in Mg-Sn powder mixture using non-isothermal differential scanning calorimetry

The non-isothermal heating process of Mg-Sn powder mixture was studied by differential scanning calorimetry(DSC) technique and the synthesis kinetics of Mg2Sn was evaluated by the model-free and model-fitting methods.The activation energy and conversion function of Mg2Sn synthesis reaction are calculated to be 281.7 kJ/mol and g(α)=[-ln(1-α)] 1/4,respectively.The reaction mechanism of 2Mg+Sn→Mg2Sn under non-isothermal condition is regarded as "nucleation and growth" .During the non-isothermal heating process,the phase transformation occurred in the Mg-Sn powder mixture was analyzed by XRD and the microstructure evolution of Mg2Sn was observed by optical microscopy,which is in good agreement with the reaction mechanism of 2Mg+Sn→ Mg2Sn deduced from the kinetic evaluation.

Measurement of Crystallinity of Acrylic Copolymer by Swelling Differential Scanning Calorimetry

In this paper the measurement of crystallinity(C)ofacrylic copolymer(PAC),by Swelling Differential Scan-ning Calorimetry(SDSC)is discussed.Common DSC isonly used for measuring the crystallinity of polymers withmelting point,(T_m),below their decomposition temper-ature,(T_d).As temperature rises,polymers with swell-ing agent added become swollen and dissolved,goingthrough whole process of breaking solid structures.Thus,SDSC makes it possible to measure the crystallini-ty of polymers even with T_d below T_m.But the C mea-sured by WAXD and the total endothermal melting(swelling)heat in SDSC thermograms,(△H_l),are notlinearly correlated.It has been found that,instead of the△H_l,△H_l’obtained from the △H_l by subtracting the en-dothermal heat,△H_l,and the C measured by WAXDare linearly correlated.On the basis of this linear rela-tion,the unknown C of another PAC sample is measuredby SDSC.The result is in good accordance with thatmeasured by WAXD.

Studies of the Energy Release of Mitochondria from Sporophyte Cytoplasmic Male Sterile Rice by Differential Scanning Calorimetry

The differential scanning calorimetric (DSC)curves of the mitochondria isolated from two varieties of sporophyte cytoplasmic male sterile and their fertile lines of Yie Bai and Ma Xie type rice have been determined. The curves show that the energy is released continuously as temperature rise to 70℃. Some thermodynamic and kinetic parameters of the energy release of the mitochondria have been obtained. The presented results showed that the mitochondria from cytoplasmic male sterile rice released more heat and they had higher energy barrier, less rate, and more complicated mechanism than that of their fertile lines in the energy release process.

Comparison between Glass and Stainless-Steel Vessels in Differential Scanning Calorimetry Estimation

Differential scanning calorimetry (DSC) provides easy screening for thermal hazard evaluation. Here, we investigate the difference between using glass and stainless-steel vessels on the DSC measurement of exothermic decomposition energy (QDSC) for 41 chemical substances (containing nitro, halogen, peroxide, and sulfur groups, and hydrazine bonds). Two borosilicate glass vessels (capillary and ampule) and one stainless-steel vessel were used. All QDSC values obtained were investigated with reference to the permissible fluctuation range specified by the ASTM (American Society for Testing and Materials) international Both glass vessels produced very similar QDSC values, despite different sample scales. The QDSC values obtained with the glass vessels were generally roughly within the variation tolerance range of the stainless-steel vessel. Notable exceptions were halogen- or sulfur-containing compounds;these exhibited smaller QDSC values with glass vessels in almost all cases. We will investigate whether certain structures in compounds react with stainless steel. The vessel material choice is crucial in evaluating the true reactivity of a substance.

Application of Single Scan Differential Scanning Calorimetry Technique for Determination of Kinetic Parameters of Crystallisation in Se-Sb-Ag

A single scan has been performed in Differential Scanning Calorimetry (DSC) at a heating rate of 15oC/min under non-isothermal conditions to investigate the crystallization kinetics of glassy Se90Sb10-xAgx alloys (where x = 2, 4, 6, 8). For this purpose, Handerson’s theory based on non-isothermal method for thermal analysis of single-scan DSC data has been used. The activation energy of crystallization and order parameter has been determined and composition dependence of these parameters has been discussed.

Thermal Diffusivity and Thermal Conductivity of Epoxy-Based Nanocomposites by the Laser Flash and Differential Scanning Calorimetry Techniques

Nanocomposites were fabricated by using a commercial two part epoxy as a matrix and multiwalled carbon nanotubes, graphite fibers and boron nitride platelets as filler materials. Multiwalled carbon nanotubes (MWCNTs) that were produced by chemical vapor deposition were found to produce nanocomposites with better thermal diffusivity and thermal conductivity than the MWCNTs that were produced by the combustion method. Compared to the MWCNTs produced by both methods and graphite fibers, boron nitride produced nanocomposites with the highest thermal conductivity. Specific heat capacity was measured by using differential scanning calorimetry and thermal diffusivity was measured by using the laser flash.

New method for analyzing recrystallization kinetics of deformed metal by differential scanning calorimeter

The drawn copper wires have been analyzed by differential scanning calorimeter(DSC) and a new method, which uses DSC measurements to determine the Johnson-Mehl-Avrami-Kolmogorov(JMAK) exponent via introducing Arrhenius behavior and modifying the baseline of DSC curves, has been proposed. The results show that JMAK exponent and recrystallization activation energy of the drawn copper wires with a strain of 2.77 are about 2.39 and 125 k J/mol, respectively. The line linking the tangency points of DSC curve hypotenuse can be used as the baseline when calculating recrystallization fraction. The JMAK exponent obtained by the DSC method is in a good agreement with that obtained by microhardness measurements. Compared to traditional methods to measure the exponent, the proposed method is faster and less labor intensive.

Application of differential scanning calorimetry to study the interpretation on herbal medicinal drugs:a review

Background:Differential scanning calorimetry as a method of investigating and monitoring the kinetics of herbal medicinal plants.Some instrumental and experimental aspects are discussed.Methods:A brief survey is made of herbal medicinal plants and results of differential scanning calorimetry studies are reviewed and this discussion is presented the effects of the instrumental conditions like heating rate and the sample conditions like sample particle size,sample mass,sample purity,sample stability in the melting region and property of impurities.Conclusion:This study suggests that application of differential scanning calorimetry to study the interpretation on herbal medicinal drugs.

基于特级初榨橄榄油两种不同特性的DSC掺假分析方法研究

该文基于油脂物理特性与氧化稳定性2种特性,利用差示扫描量热法(differential scanning calorimetry,DSC)对市面上常见的特级初榨橄榄油(extra virgin olive oil,EVOO)中大豆油掺假问题进行研究。在物理特性方面,采用DSC冷却曲线来分析EVOO掺假。随着大豆油掺假比例升高,油样在-40~-60℃结晶焓值ΔH由EVOO的29.78 J/g减小为40%掺假混合油的6.133 J/g,对EVOO质量比构建的一元回归方程Y=57.556X-28.44(R2=0.997)。在氧化稳定性方面,氧化温度160℃下,不同油样诱导氧化时间随大豆油掺假比例上升逐渐变短,由EVOO的25.8 min逐渐减小为40%掺假混合油的17.8 min,Y=-19.4X+25.64(R^(2)=0.996),掺假模型相关性较好。这2种DSC检验掺假分析方法都能有效鉴别EVOO中大豆油的掺假且各有特点,可根据实际情况选取合适的方法更好处理EVOO掺假问题。

加热氧化对山茶油热力学及流变学特性的影响

目的探究加热氧化对山茶油热力学及流变学特性的影响。方法山茶油经加热氧化处理后,运用差示扫描量热技术(differential scanning calorimetry,DSC)、旋转流变技术,研究其DSC氧化稳定性,熔融结晶特性及黏度随剪切速率、温度变化等特性。结果山茶油加热时间越长,其DSC热力学氧化稳定性越低,当加热120 min后较初始山茶油的氧化起始温度降低了8.3℃,加热氧化后它的熔融温度及熔融焓降低,主要结晶峰消失。山茶油加热氧化后流动性变差,表现为黏度升高,加热120 min的山茶油较初始山茶油黏度提高了2.8倍,山茶油氧化程度越高,其黏度随温变化的速率越快。结论加热氧化降低了山茶油的热力学稳定性及流变学稳定性,本研究为山茶油精深加工的热力学性能及流变性能提供了一定的理论支撑。

核医学检查在评估中低危分化型甲状腺癌患者术后淋巴结转移中的价值

目的探讨中低危分化型甲状腺癌患者术后刺激状态下甲状腺吸碘率、甲状腺功能及残留甲状腺131I最大计数评估发生淋巴结转移的临床价值。方法随机选取2016年1月—2018年12月就诊于我院临床资料齐全的中低危分化型甲状腺癌术后并欲行131I治疗的182例分化型甲状腺癌(DTC)患者,收集所有患者甲状腺吸碘率、甲状腺功能、颈部超声、131I全身扫描及颈部SPECT/CT断层显像资料。结合淋巴结术后病理、颈部超声、颈部SPECT/CT断层显像及临床随访来最终确定颈部淋巴结转移情况。分析甲状腺吸碘率、功能、131I最大计数诊断淋巴结转移的相关因素。结果二元Logistic回归分析结果显示,中低危分化型甲状腺癌颈部淋巴结转移与术后刺激状态下吸碘率(P=0.048)、Tg(P=0.048)、131I最大计数(P=0.049)有关,与TSH(P=0.256)、FT3(P=0.516)、FT4(P=0.827)、TgAb(P=0.351)、TPOAb(P=0.389)无关。将吸碘率、Tg、131I最大计数对转移进行ROC处理,三者中吸碘率诊断效能最高,131I最大计数效能最差,吸碘率、Tg的临界值分别为1.5、5.28时对评估淋巴结转移有统计意义,131I最大计数临界值为727,但无统计学意义。通过偏相关分析显示,吸碘率、TSH、FT3、FT4、TgAb均与131I最大计数有关,其中吸碘率、FT3、FT4与131I最大计数呈正相关,TSH、TgAb与131I最大计数呈负相关(P<0.05)。结论吸碘率、Tg、131I最大计数对淋巴结转移有一定评估价值;吸碘率、FT3、FT4值越高,提示131I最大计数越高;TSH、TgAb值越高,对应131I最大计数水平越低。

超声在线监测不饱和聚酯树脂固化过程及其动力学行为

为探索不饱和聚酯树脂(UPR)固化体系在不同温度下的超声振幅变化规律,采用超声波穿透技术对UPR固化过程进行在线监测,获得声速、储能模量、松弛时间、凝胶时间等动力学参数变化规律,并得到固化反应动力学方程。结果表明:温度越高,声速与储能模量变化越快,且最终数值也越大,而固化松弛时间与凝胶时间随温度增加而缩短;此外,超声法与差示扫描量热法(DSC)得到的固化度曲线变化高度一致,通过2种方法所得到的反应活化能分别为38.14 kJ/mol和45.3 kJ/mol;最终,通过DSC法确定了UPR固化反应动力学级数为0.92。总之,超声法与DSC法2种方法相互结合,不仅证明了超声结果的准确性,也为UPR固化过程提供一种精准的在线监控技术和量化方法,从而为UPR生产过程提供理论指导。

MRI平扫及增强扫描对肾癌病理亚型的鉴别价值分析

目的分析MRI平扫及增强扫描对肾癌病理亚型的鉴别价值。方法回顾性分析2017年2月至2023年4月安阳市人民医院收治的114例肾癌患者的临床资料,所有患者均经病理检查证实为肾癌且治疗前均接受过磁共振成像(MRI)平扫及增强扫描。比较各病理亚型肾癌患者MRI平扫及增强扫描表现,并以病理结果为“金标准”,评价MRI平扫及增强扫描在肾癌病理亚型中的鉴别价值。结果pRCC和cRCC患者ADC值低于ccRCC患者(P<0.05);cRCC患者T1WI和T2WI平扫低、等信号占比高于ccRCC和pRCC患者(P<0.05),混杂信号占比低于ccRCC和pRCC患者(P<0.05)。pRCC和cRCC患者不均匀强化占比低于ccRCC患者(P<0.05),且cRCC患者不均匀强化占比低于pRCC患者(P<0.05);不同病理亚型强化程度分布差异有统计学意义(P<0.05),ccRCC以重度强化为主,pRCC以轻中度强化为主,cRCC均为轻度强化患者;pRCC和cRCC患者皮质期、实质期、延迟期信号强度变化均低于ccRCC患者(P<0.05),且pRCC患者以上各期信号强度变化均低于cRCC患者(P<0.05)。MRI平扫及增强扫描联合鉴别ccRCC的灵敏度、准确度均高于单项鉴别(P<0.05);MRI平扫及增强扫描联合鉴别pRCC的特异度、准确度均高于单项鉴别(P<0.05),灵敏度高于MRI平扫单项鉴别(P<0.05);MRI平扫及增强扫描联合鉴别cRCC准确度高于单项鉴别(P<0.05)。结论不同病理亚型肾癌患者的MRI平扫及增强扫描表现存在差异,且MRI平扫及增强扫描联合鉴别肾癌病理亚型的价值较高。

多模态高场MRI乳腺扫描对乳腺良恶性病变的诊断价值

目的 分析多模态高场磁共振成像(MRI)乳腺扫描诊断乳腺良恶性病变的临床价值。方法 收集2022年1月至2023年12月于河南科技大学第二附属医院进行乳腺MRI检查的79例乳腺患者的临床资料,所有患者入院后均接受高场MRI轴位T1加权成像(T1WI)、压脂T2加权成像(fs-T2WI)、扩散加权成像(DWI)、表观弥散系数(ADC)、动态对比增强(DCE),并将扫描的图像传至配套的后处理软件工作站建立病灶感兴趣区的动态增强曲线(DCE-TIC)及最大强度投影(MIP)图像、分析多模态高场MRI乳腺扫描在诊断乳腺良恶性病变方面的临床价值。结果 以组织病理学检查结果作为金标准,79例患者中发现81个病灶,其中良性病变44个,恶性病变37个,有2例患者存在2个病变并存的情况,1例是左乳纤维腺瘤,右乳微小粘液癌,1例是左乳发现2个病变,血管平滑肌瘤和叶状肿瘤并存。磁共振平扫、动态对比增强扫描和多模态高场MRI乳腺扫描诊断恶性病变的灵敏度分别为72.97%、86.49%、94.59%,特异度分别为54.55%、59.09%、81.82%,准确度分别为62.96%、71.60%、87.65%,约登指数分别为0.28、0.46、0.76。其中多模态高场MRI乳腺扫描诊断乳腺恶性病变效能最高,灵敏度、特异度、准确度及约等指数分别为94.59%、81.82%、87.65%,0.76,高于单一做乳腺磁共振平扫或单做动态对比增强成像。结论 多单一做乳腺平扫或DCE检查都有一定的不足,多模态高场MRI乳腺扫描诊断乳腺良恶性病变的诊断效能较好,对乳腺恶性病变诊断的准确性较高,对乳腺良恶性病变的诊断具有较高的临床价值。

基于强流脉冲离子束的中子辐照模拟装置及评价技术

依据高能原子辐照与中子辐照的初级离位原子(PKA)能谱相似性,基于TEMP-6M型强流脉冲离子束(HIPIB)系统,研发了一种中子辐照模拟装置,该装置以磁绝缘离子二极管伴生的强流脉冲二次电子束流实现0.1 MeV以上高能离子的高效率中和,获得动能为0.1~1 MeV、脉冲宽度为120~160 ns、脉冲辐照剂量为1012~10^(15)n/cm^(2)的强流脉冲原子或混合束,原子占比为85%~100%。通过辐照缺陷原位差热分析方法,快速确定材料缺陷数量、密度及dpa损伤速率等抗中子辐照性能评价指标。以核级AISI 304奥氏体不锈钢为例,计算PKA相似性定标曲线,采用220~280 keV的C原子等效1.8~2.3 MeV中子进行辐照模拟,调节名义束流能量密度0.5~4 J/cm^(2),实测辐照剂量范围为0.46×10^(13)~8.55×10^(13)n/cm^(2),热分析确定Frenkel缺陷密度为1.99×10^(16)~2.90×10^(17)/cm^(2),外推预测奥氏体不锈钢在1021n/cm^(2)中子剂量条件下的辐照损伤为500 dpa量级,适用于核电厂结构材料60年服役寿期评价需求。

基于视网膜结构改变的机器学习对早期帕金森病诊断的预测价值研究

背景帕金森病(PD)的诊断主要以临床症状为主,缺乏正确诊断的客观方法。目前已有关于视网膜结构改变作为PD早期诊断的生物标志的研究,但基于视网膜结构改变的机器学习对预测早期PD的研究尚少。目的基于视网膜结构改变的特征构建机器学习模型,探索其在早期PD诊断中的预测价值,及探讨不同机器学习算法对PD早期诊断的准确性。方法选取2021年10月—2022年9月在河南省人民医院神经内科门诊就诊和住院治疗的年龄40~70岁的PD患者49例(PD组),并选取来医院体检的年龄及性别相匹配的39名健康者(健康对照组)为研究对象。所有研究对象行扫频源光学相关断层扫描和扫频源光学相干断层扫描血流成像检查,并定量分析黄斑区视网膜的厚度和血管密度。将88例受试者按7∶3的比例随机分为训练集62例和验证集26例,选择PD组与健康对照组差异有统计学意义的变量作为纳入机器学习模型的特征变量,并在训练集中分别构建Logistic回归(LR)、K-近邻算法(KNN)、决策树(DT)、随机森林(RF)和极端梯度提升(XGboost)模型。采用受试者工作特征(ROC)曲线下面积(AUC)、准确度、灵敏度和特异度评价基于视网膜改变的机器学习模型对早期PD诊断的预测价值。结果与健康对照组相比,PD组患者浅层毛细血管的上方外圈(A6)、颞侧外圈(A7)、下方外圈(A8)以及鼻侧外圈(A9)密度减少,视网膜层的上方内圈(A2)、颞侧内圈(A3)、下方内圈(A4)、鼻侧内圈(A5)、A6~A9厚度,节细胞复合体层的A9厚度,神经纤维层的A7厚度,视网膜外层的A2和A4~A9厚度变薄(P<0.05)。视网膜层A2厚度(OR=0.781,95%CI=0.659~0.926)、视网膜层A3厚度(OR=1.190,95%CI=1.019~1.390)、视网膜外层A2厚度(OR=0.748,95%CI=0.603~0.929)、视网膜外层A6厚度(OR=2.264,95%CI=1.469~3.490)、视网膜外层A8厚度(OR=0.723,95%CI=0.576~0.906)以及神经纤维层A7厚度变薄(OR=0.592,95%CI=0.454~0.773)及浅层毛细血管A7密度减少(OR=1.966,95%CI=1.399~2.765)为早期PD发生的独立危险因素(P<0.05)。将上述变量纳入并构建机器学习模型,结果显示,构建的5个模型中,LR模型整体性能最高,其AUC为0.841,而DT模型的准确度最高,其准确度为0.846。结论基于视网膜特征的机器学习模型可准确的预测早期PD,其中,DT模型对早期PD诊断具有较高的准确度。

可降解生物基含酯键环氧树脂的固化动力学研究

采用非等温差示扫描量热(DSC)法研究了可降解生物基含酯键环氧树脂固化动力学,分别建立了n级反应动力学模型、自催化模型以及结合n级反应和自催化模型的分段模型,并将模型预测值与实验数据进行了对比分析。结果表明,n级反应模型与实验曲线的偏差较大,自催化模型与实验曲线变化趋势基本一致,但仍然存在一定偏差,而结合两者的分段模型与实验曲线吻合较好,表明分段模型能更准确地描述该环氧树脂体系的固化反应过程,为其树脂基复合材料固化成型工艺条件优化提供理论指导。