杜邦工程料的實驗

1、杜邦工程塑料測試及分析實驗室能力介紹Testing & AnalyticalLaboratory CapabilityIrene Chen 測試及分析實驗室介紹Introduction of Testing&Analytical Laboratory單項測試能力總攬測試項目及儀器簡介綜合測試服務(wù)簡介綜合測試服務(wù)實例Testing capabilities Overview Testing Instrument& Items Problem Solving competence Examples 機(jī)械性能測試Mechanical 拉伸性能-拉伸強(qiáng)度拉伸強(qiáng)度,模量模量,伸長

2、率 Tensile-strength, Modulus, strain彎曲性能-彎曲強(qiáng)度彎曲強(qiáng)度,模量模量。Flexural-strength, Modulus沖擊強(qiáng)度Impact strength邵氏硬度邵氏硬度(僅彈性體僅彈性體Shore Hardness( for elastomer 彈性體直角撕裂強(qiáng)度Tear strength( for elastomer 物理性能測試Physical密度/比重Density/ Specific gravity灰分ash 粘度特性Viscosity熔體流動速率Melt Flow Rate(MFR熔體粘度Melt Viscosity(MV溶液粘度-僅尼龍

3、材料Relative viscosity-for Nylon only 熱分析Thermal Analysis 熔點等Melting Point etc熱變形溫度Deflection Temperature Under Load燃燒性能Flammability灼熱絲燃燒實驗glow Wire flammabilityUL94老化性能Ageing熱老化,油老化油老化,冷凍液老化Heat Ageing,Oil Ageing, LLC ageing 恒溫恒濕老化( 30-100C,0-100%RH Temperature-Humidity Chamber光學(xué)分析Optical紅外光譜FTIR顯微切片

4、分析Polarized Microscope 體視顯微分析Stereo Microscope掃描電鏡SEM 其它測試Others 水分含量Moisture Content單項測試-機(jī)械性能測試Single Test-mechanicalISO 34-15直角撕裂強(qiáng)度tear strength ISO 179-1 :20104簡支梁沖擊強(qiáng)度Charpy Impact ISO 180 :20003懸臂梁沖擊強(qiáng)度Izod impact ISO 178 :20102彎曲性能flexuralISO 527-1,-2 :20121拉伸性能tensile 方法method 項目itemISO 8686邵氏硬

5、度,A&D shore hardness ISO294-47成型收縮率molding shrinkage拉伸性能測試 標(biāo)準(zhǔn)試樣在沿其縱向主軸以恒速拉伸直到斷裂或直到應(yīng)力或應(yīng)變達(dá)到某預(yù)定值或應(yīng)變達(dá)到某預(yù)定值,測量在這一過程中試樣所受的負(fù)荷和伸長率常用啞鈴型常用啞鈴型(或狗骨頭型或狗骨頭型的試樣用于拉伸性能測試彈性模量E t :在彈性范圍的線性比例極限內(nèi)在彈性范圍的線性比例極限內(nèi),材料所受的應(yīng)力與相應(yīng)的應(yīng)變的比拉伸性能常用術(shù)語屈服強(qiáng)度y :在應(yīng)力-應(yīng)變曲線上應(yīng)變曲線上,第一個屈服點所對應(yīng)的應(yīng)力第一個屈服點所對應(yīng)的應(yīng)力。斷裂強(qiáng)度b :在應(yīng)力-應(yīng)變曲線上應(yīng)變曲線上,試樣斷裂時所對應(yīng)的應(yīng)力試樣斷

6、裂時所對應(yīng)的應(yīng)力。拉伸強(qiáng)度t :在拉伸試驗中直到斷裂為止在拉伸試驗中直到斷裂為止,試樣所承受的最大拉伸應(yīng)力試樣所承受的最大拉伸應(yīng)力。屈服/斷裂伸長率y %/b %:試樣在屈服/斷裂時對應(yīng)的拉伸應(yīng)變典型應(yīng)力-應(yīng)變曲線 屈服強(qiáng)度屈服伸長率拉伸強(qiáng)度斷裂伸長率應(yīng)力應(yīng)變曲線應(yīng)變曲線(Stress-strain curve A-脆性材料脆性材料,如Zytel 70G33B ,C-具有屈服點的韌性材料具有屈服點的韌性材料,如Zytel ® 101L, Delrin® 500PD-無屈服點的韌性材料,如Hytrel ®Zytel® 101L DAMDelrin®

7、; 500PHytrel ® DYM350Zytel ® 70G33拉伸應(yīng)力及彈性模量的計算 =應(yīng)力 M P a 應(yīng)變,%Att比例極限A B彈性極限B C屈服點C DD斷裂點D =ForceSectionMPaL -L L = % L L= =MPaE = 拉伸彈性模量tt tt=F * LS * L0LLF SectionForceL彎曲性能 彎曲性能試驗彎曲試驗主要用來檢驗材料在經(jīng)受彎曲負(fù)荷作用時的性能受彎曲負(fù)荷作用時的性能。常用采用簡支梁法三點彎曲試驗采用簡支梁法三點彎曲試驗,試驗時將試樣置于兩支座上驗時將試樣置于兩支座上,并在兩支座的中點施加一集中負(fù)荷兩支座的中點

8、施加一集中負(fù)荷,使試樣產(chǎn)生彎曲應(yīng)力和變形力LHF規(guī)定撓度規(guī)定撓度:等于試樣厚度的1.5倍的撓度彎曲性能常用術(shù)語撓度撓度:彎曲過程中彎曲過程中,試樣跨度中心的頂面或底面偏離原始位置的距離彎曲強(qiáng)度彎曲強(qiáng)度:在達(dá)到規(guī)定撓度值時或之前在達(dá)到規(guī)定撓度值時或之前,負(fù)荷達(dá)到最大值時的彎曲應(yīng)力(見下圖曲線a 和b 彎曲模量彎曲模量:在線性形變范圍內(nèi)在線性形變范圍內(nèi),彎曲應(yīng)力差與對應(yīng)的應(yīng)變的比值定撓彎曲強(qiáng)度定撓彎曲強(qiáng)度:在規(guī)定撓度值時的彎曲應(yīng)力在規(guī)定撓度值時的彎曲應(yīng)力。彎曲應(yīng)力-應(yīng)變曲線曲線a: 試樣在屈服前斷裂試樣在屈服前斷裂。如70G33曲線b 試樣有最大彎曲應(yīng)力,然后在規(guī)定撓度Sc到達(dá)到前斷裂.曲線c 試

9、樣既無最大彎曲應(yīng)力應(yīng)力,也不在規(guī)定撓度前斷裂如Hytrel 350BK 規(guī)定撓度 彎曲應(yīng)力及模量的計算S t r e s s M P a =ssE s = ss s力LHFW = 試樣寬度D = 撓度F * L 34 * W * H 3 * DE = 彎曲模量c = MPaccc = =c6*D*H L 2= 彎曲應(yīng)變cMPa =c3*F*L 2 * W * H 2= 彎曲應(yīng)力c沖擊性能試驗是在沖擊負(fù)荷作用下測定材料的沖擊強(qiáng)度沖擊性能試驗是在沖擊負(fù)荷作用下測定材料的沖擊強(qiáng)度。它用于評價材料抵抗沖擊破壞的能力或判斷材料的脆性或韌性程度沖擊性能測試擺錘式?jīng)_擊試驗方法可分為常用的沖擊強(qiáng)度測試方法有擺

10、錘式?jīng)_擊試驗使用安裝在標(biāo)準(zhǔn)化沖擊試驗機(jī)上的標(biāo)準(zhǔn)化的擺錘擺錘式?jīng)_擊試驗使用安裝在標(biāo)準(zhǔn)化沖擊試驗機(jī)上的標(biāo)準(zhǔn)化的擺錘,測定其擺動一次沖斷材料的標(biāo)準(zhǔn)試樣所消耗的能量簡支梁沖擊強(qiáng)度簡支梁沖擊強(qiáng)度,ISO179, ASTM D6110懸臂梁沖擊強(qiáng)度, ISO180, ASTM D256.擺錘式?jīng)_擊試驗落球沖擊試驗Charpy 簡支梁沖擊試驗示意 簡支梁沖擊試驗ISO 179, ASTM D6110 懸臂梁沖擊Izod 懸臂梁沖擊試驗示意ISO179 沖擊強(qiáng)度的表示ISO179-1/ 1 e A測試標(biāo)準(zhǔn)試樣類型,1沖擊方向,e指試樣平放缺口類型,A-A型缺口沖擊方向U-無缺口沖擊方向ISO180/ A測試標(biāo)

11、準(zhǔn)缺口類型,A-A型缺口U-無缺口ISO180 沖擊強(qiáng)度的表示 塑料材料的硬度Hardness of plasticsFShore: 1, 3 or 15 secMethod Standard Weight Needle MaterialShore A ISO 868 1 Kg Area Ø 0,79Rubber, very soft plasticsShore D ISO 868 5 Kg Needle R 0,1Soft plastics and elastomers Rockwell M ISO 2039100 Kg Ball Ø 6,35PlasticsRockwe

12、ll R ISO 203960 Kg Ball Ø 12,7PlasticsRockwell L ISO 203960 Kg Ball Ø 6,35Plastics塑料材料的硬度Hardness of plastics 方法Method 項目Item4 熔體粘度Melt viscosityISO 11333 熔體流動速率MFR ISO 3072 粘數(shù)viscosity Number ASTM D7891 相對粘度relative viscosity ISO 11443單項測試-粘度測試viscosity measurement粘度是影響聚合物的機(jī)械性能及加工性能的一個非常重

13、要的性質(zhì)粘度是影響聚合物的機(jī)械性能及加工性能的一個非常重要的性質(zhì)。聚合物的粘度越高聚合物的粘度越高,力學(xué)性能越好力學(xué)性能越好。Viscosity is very important to mechanic and processing properties of polymer, Higher viscosity, Higher mechanic properties僅尼龍溶液粘度(僅尼龍Solution viscosity(Zytel only把聚合物溶解在溶劑中,制成特定濃度的溶液,測定溶液的粘度。Dissolve the polymer in suitable solvent, and

14、prepare its thinner solution, measure the viscosity of the solution溶液的粘度取決于聚合物分子量的高低。分子量高,溶液的粘度高solution viscosity depends on molecular weight of polymer, highermolecular weight, higher solution viscosity25溶液粘度之相對粘度-Solution viscosity-relative viscosity對尼龍材料,通常我們測定溶液的相對粘度(relative viscosity,RV 或粘數(shù)(v

15、iscosity number,VNFor nylon material, relative viscosity (RV, ASTM standard or viscosity number (VN, ISO standard are commonly used相對粘度的測量-ASTM D789Measurement of relative viscosity把2.200g 尼龍樹脂加入到20ml的25的90%的甲酸(96%的濃硫酸中,制得重量百分比為8.4%的尼龍-90%甲酸(或96%硫酸溶液,測定此溶液流經(jīng)粘度管的時間。at a temperature of 25,Dissolve 2.2

16、00g nylon resin into 20ml 90% formic acid or96% sulphuric acid , then we get a Nylon-acid solution, measure the time thesolution flow through the viscometer.26溶液粘度之粘數(shù)Solution viscosity-viscosity number粘數(shù)的測量-ISO307Measurement of viscosity number把尼龍樹脂加入到25的96%的濃硫酸中,制得濃度為0.005g/ml的尼龍-96%硫酸溶液,測定此溶液流經(jīng)粘度管

17、的時間。at a temperature of 25,Dissolve nylon resin into sulfuric acid with a weightconcentration of 96%, then we get a Nylon-96% sulfuric acid solution with aconcentration of 0.005g/ml, measure the time the solution flow through theviscometer.27熔體流動速率熔體流動速率(熔融指數(shù)Melt mass-flow rate, MFRmelt index(MI orm

18、elt flow index(MFI are widely used在規(guī)定溫度下,塑料熔體在固定載荷下流過口模的速率單位:g/10minrate of extrusion of a molten resin through a die of specified length and diameter under prescribed conditions of temperature,load and piston position in the barrel of an extrusion plastometer,the rate being determined as the mass e

19、xtruded over a specified time28砝碼weight柱塞plunge 熔體melt口模die料筒Barrel Heater隔熱保護(hù)層Heat Insulation layer 熔體流動速率儀Extrusion plastometer熔體流動速率測定Measurement of MFR 熔體粘度指塑料融熔成液體狀態(tài)后的粘度melt viscosity is the viscosity of plastic after meltingit reflect the flowability of plastics melt毛細(xì)管流變儀Capillary Rheometer31

20、熔體粘度對溫度的依賴性MV Vs Temperature溫度升高 , 熔體粘度下降MV decreased with theincrease of melttemperatureShear rate=1000 1/s 32熔體粘度對剪切速率的依賴性MV Vs shear rate剪切速率升高 , 熔體粘度下降MV decreased with theincrease of shear rate 水分含量對熔體粘度的影響MV Vs moisture content 剪切速率粘 度含水量越高,粘度越小Higher moisturecontent, smallerMV34單項測試 -熱分析 Ther

21、mal AnalysisDSC(DifferentialScanning Calorimeter 通過測量聚合物的熱焓隨溫度的變 化 , 得到聚合物玻璃化轉(zhuǎn)變溫度 得到聚合物玻璃化轉(zhuǎn)變溫度, , 融熔溫度 融熔溫度, , 結(jié)晶度 結(jié)晶度, , 比熱等熱性能參數(shù) 比熱等熱性能參數(shù)。 。 The DSC measures the specific heat of the polymer as a function of the temperature , typically the main endotherm /exotherm reactions occurring during heatin

22、g /cooling the polymers which are the melting /freezing and eventual glass transition temperatures.聚合物的性能受溫度的影響很大 聚合物的性能受溫度的影響很大, , 熱分析方法使我們了解溫度變化時聚合物發(fā) 生的結(jié)構(gòu)變化 生的結(jié)構(gòu)變化, , 它解釋了為什么聚合物在不同溫度下的性能表現(xiàn)不同 它解釋了為什么聚合物在不同溫度下的性能表現(xiàn)不同。 。 Polymers are highly influenced by the temperature.thermal analysis allow to unde

23、rstand Phenomenon taking place in the structure of the polymer Explains the difference of behavior as a function of the temperature at which they are exposed.35 DSC Used in Material Analysis FunctionGet the transition temperatures (such as Tg and Tm related to thermal behaviors of the materials. Wha

24、t can be got?For crystalline polymers1.1 Melting temperature or melting point (Tm or MP1.2 Crystallization temperature( Tc1.3 Relative crystallinity.1.4 Crystallization extent-sufficient or insufficientAmorphous material2.1 Glass transition temperature (Tg.Note :Tg might be interfered by the vaporiz

25、ation of absorbed water around 100 C degree.單項測試-熱分析Thermal Analysis參考方法Method ISO 11357典型的DSC 分析曲線Typical DSC curveTg: 玻璃化轉(zhuǎn)變溫度Tc :結(jié)晶溫度Tm: 熔點TemperatureHeat flowMelting Point (DSC通常我們?nèi)〉诙渭訜釙r曲線的峰值為熔點 Cold crystallization peak,Hc=2.298J/g Melting peak,Hm=20.96J/g% Crystallinity = Hm Hc / (Hm ° wt

26、 % of PET resin in formulation*100%= (20.96-2.298/(140.1*60%*100%= 22%Recrystallization and Calculation of crystallinity By DSC-Example#1 for Rynite ® RE19051Cold crystallization is typical for Rynite® PET and Zytel® HTN 51G series Too low mold temperature is the main cause of recryst

27、allizationTGA(Thermo gravimetry Analysis TGA AnalysisFunctionMaterial Thermal stability evaluationAsh content analysisAnalysis1. Run heating at a certain heating rate and get weight loss curve;2. Weight loss might caused by vaporizing, decomposing et al.TGA chartCarbon residue Temperature of deflect

28、ion under load熱變形溫度測試Commonly called :HDT (Heat Distortion TemperatureorDTUL (Deflection Temperature Under LoadA standard test specimen is subjected to three-point bending under a constant load and specific support span to produce a 1.8MPa or 0.45MPa flexural stresses,the temperature is raised at 12

29、0o C/hour ,and the temperature at which the standard deflection corresponding to the specified increase in flexural strain occurs is measured.把標(biāo)準(zhǔn)試樣放在規(guī)定跨距的支座上把標(biāo)準(zhǔn)試樣放在規(guī)定跨距的支座上,并在兩支座的中點處施加規(guī)定的負(fù)荷并在兩支座的中點處施加規(guī)定的負(fù)荷,形成三點簡支梁式靜彎曲成三點簡支梁式靜彎曲,使試樣形成1.82MPa 或0.45MPa 的表面彎曲應(yīng)力的表面彎曲應(yīng)力,把受到負(fù)荷的試樣浸在導(dǎo)熱的液體介質(zhì)中受到負(fù)荷的試樣浸在導(dǎo)熱的液體介質(zhì)中

30、,以120o C/小時的速率升溫小時的速率升溫,當(dāng)試樣中點的變形量達(dá)到規(guī)定值時所對應(yīng)的溫度點的變形量達(dá)到規(guī)定值時所對應(yīng)的溫度,就是材料的熱變形溫度就是材料的熱變形溫度。Schematic Figure of HDT testing Typical Chart of HDT 單項測試-紅外光譜(FTIR分析FTIR analysis紅外光照射到物質(zhì)后被吸收紅外光照射到物質(zhì)后被吸收、透射或反射形成的譜線It is the spectrum of infra red light absorbed/transmitted/reflected by material N-H stretch vibration1550cm -1,overtoneC=O stretch vibrationN-H,out surface swinAmid