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1、声 明 本讲稿中引用的图、表、数据全部取自公开发表的书籍、文献、论文，而且仅为教学使用，任何人不得将其用于商业目的。磁性测量仪器篇 之三PPMS的介绍多功能物性测量系统介绍第 1 单元 PPMS主机硬件共44页该单元的内容vPPMS14H的总体结构vPPMS的温度控制v杜瓦液氦液氮vPPMS的磁场控制v样品室样品架选件vPPMS14H的附属设备温度、磁场平台通用检测端口功能扩展需要关注的内容1.主机的功能：磁场、温度、位置2.如何控制：温度、磁场、位置、样品室气氛3.如何实现多功能：选件种类、功能、连线4.如何安装取放样品：通用工具、专用工具PPMS14H基本系统的技术指标v温度基本系统：1.
2、8 K 400 KHe3系统：0.35 K 350 K高温炉：300 K 800 K控温模式：Fast Settle、No Oshoot、Sweeptypical 12 K/minACMS:1.8 K 350 KPPMS14H基本系统的技术指标v温度：均匀区及稳定性10 cm纯铜制温度均匀区Typical Accuracy：0.5Stability：0.2，when 10 K 0.02，when 10 KPPMS14H基本系统的技术指标v磁场基本系统：14 T杂散磁场屏蔽：Stray Field Shield超导磁体剩余磁场校正：Ultra Low Field9.2 Oe/sec 42.6 O
3、e/sec变场模式：Linear、Persistent、Driven、Oscillate5 Oe50 mOeMagnet Reset(Quench):InvalidPPMS14H基本系统的技术指标v磁场：均匀区磁场均匀区：在磁体中心的5.5 cm范围内：0.1(14 T)B/I：1492.35 Oe/A；（6.7008 A 1.0 T）Magnet Inductance：35 H；Charge Voltage：LoB 1.0，HiB 1.0；Switch Time：Warm 20 sec，Cool 20 sec。PPMS14H基本系统的技术指标v样品台方向磁场方向：纵向（垂直于地面）水平旋转台
4、：8.512 371.442PPMS14H基本系统的技术指标v运行成本液氦：68 升（每周80升）液氮：48升（每周100升）电力：3 kVA，220 V，50 Hz其它：油脂,吸管,焊料，总体结构图杜瓦PPMS Probe计算机控制柜6000：信号控制中心6700：磁体电源6500：比热、循环制冷机7100：交流电源旋转马达、伺服马达PPMS控制框图杜瓦剖面图温度/气体控制控温样品室杜瓦充气阀清洗阀控温流量阀PPMS主机的温度检测VI80 K100 K电阻温度计铂电阻温度计Platinum ThermometerCernox温度计Negative ThermometerCoefficient
5、(NTC)1.8 K400 K液氮夹层高容量杜瓦High Capacity Nitrogen-Jacketed DewarLHe:68 litersLN2:48 liters向上杜瓦俯视图杜瓦剖面图杜瓦液氦液面 94.6 31.0 液氮夹层PPMS液氦液面指示计磁体样品室PPMS Probe磁体中心温度计、加热器液氦流阻器磁场控制过程H=H0，闭环，电源关H=Hf，闭环，电源关H=H0，电流恒定，开环H=Hf，电流恒定，闭环H=Hf，开环，调节磁场H=H0，闭环，电源电流升液氦液面与最大磁场的关系0.0 10 31 45 50 60 94.6 100 85 Full Field(14 T)Li
6、mit forHelium Fill?未知65液氦液面与可用磁场的关系（暂定）1.65以上，可以使用最高磁场 14 T2.60 65之间，可以使用最高磁场 10 T3.55 60之间，可以使用最高磁场 5 T4.50 55之间，可以使用最高磁场 1 T液氦液面必须始终保持在10以上。PPMS多参数测量测量环境平台温度、磁场通用信号采集端口选件控制端口与引线数据？样品PPMS样品室通用信号采集端口PPMS样品室通用信号采集端口样品室端口样品架端口PPMS选件控制端口与引线ACMS CoilSetHorizontal RotatorHelium 3 Insert限位PPMS选件控制端口与引线ACM
7、SULFSample TransportACMS PreamplifierMotor control to Model 6000Fluxgate CableInterface CablePPMS选件控制端口与引线ACTStandard “Y”CableACT/Helium-3 Probe CableACT/Horizontal Rotator Probe CablePPMS选件控制端口与引线HCTq-MagDSP Cable AssemblyInterface CablePPMS Head的后侧视图用于连接测量选件PPMS控制柜后面板Model 6000Model 7100Model 6500
8、Servo Motor Control硬件连接框图vUtilities Activate Option Connection DiagramActivateConfigure OptionLog PPMS DataUploadSend GPIB CommandsMagnet Error HandlingEvent LogHelium FillAvailable Options:Active Options:Option ManagerAC TransportACMSHeat CapacityHelium3Low FieldResistivityThermal TransportTorque M
9、agnetometerActivate-DeactivateConnectionDiagramsCloseMultiVuInstrument&UtilitiesActivateConfigure OptionLog PPMS DataUploadSend GPIB CommandsMagnetError HandlingEvent LogHelium FillMultiVuPPMS Status Bar_MultiVu程序温度磁场样品室MultiVuCommands:FieldImmediate Mode and Sequence Mode磁 场MultiVu_FieldMagnetic Fi
10、eldRate9.2 42.6 Oe/sec依赖于B/I电感电压Approach S c a n F i e l dS e t F i e l dLinear快No Overshoot中Oscillate慢Sweep快End ModePersistent闭环Driven(Hysteresis)开环达到设定磁场速率磁体中电流变化方式后磁场保持模式FieldMagnetic Field当前磁场变场速率PersistentDrivenSW WarmSW CoolSWTC ErrChargingDischargingIteratePersistentHoldingChrg ErrCurr ErrFai
11、lureQuenchLinearNo OvershootOscillateSweep设定磁场FieldScan FieldSpacing CodeUniform CodeH等间隔H*H CodeH2等间隔H1/2 CodeH1/2等间隔1/H Code1/H等间隔Log(H)CodeH对数等间隔FieldProcess of Setting Field_ApproachModeCharging/DischargingSet RateApproach ModeFieldtimeHolding:DrivenSwitch Warming:Persistent(20 Sec)PresentSetpoi
12、ntLinearSweep(Scan)No OShoot70%Oscillate30%Process of Setting Field_EndModeCurrent of Power SupplytimeHoldingDrivenSwitch Cooling:Persistent(20 Sec)I=0.0ISetpointSweep?LinearNo OShootOscillateSweepDriven&PersistentSet PointEnd PointDriven&PersistentMeasurement_Approach_EndModeFieldtimeHoldingDrivenP
13、ersistent ModeI=0.0ISetpointSweep(Scan)测量开始/结束tH测量开始/结束t开始/结束测量tH 0H 0H rate tCommands:TemperatureImmediate Mode and Sequence Mode温 度MultiVu_TemperatureTemperatureRate0.01 K/min20.00 K/minTypical:12.00 K/minMode or Approach Scan TemperatureSet TemperatureFast Settle快No Overshoot慢Sweep快达到设定温度速率变温方式Te
14、mperatureTemperature当前温度变温速率指 示含 义Chasing达不到设定速率Tracking按照设定速率Near确认温度稳定性Stable温度已经稳定Potops液氦储槽操作Standby关闭温度控制Unknown检修、转换Fault温度系统错误Impedfail流阻故障ImpCtrl流阻加热故障ImpCool流阻冷却故障Fast SettleNo OvershootSweep设定温度TemperatureScan TemperatureSpacingUniform CodeT等间隔1/T Code1/T等间隔Log(T)CodeT对数等间隔Temperature见本系列超
15、导量子磁强计Temperature“Complicated”ManualQuantum DesignHigh-TemperatureControl4.2 K2.2 K400 K1.8 KLow-TemperatureControl(Pot Mode)ContinuousLow-TemperatureControl(CLTC)尽量避开TemperaturePPMSMPMSPPMS的各种“Temperature”Temp(The temperature)Depending on option usedSys Temp(System temperature)Cernox or Platinum th
16、ermometerSetpointTarget temperatureCIG/CernoxLow-temperature thermometerPlat ThermHigh-temperature thermometerNeck ThermNeck thermometerSpare ThermSystem bridge channel 4 resistanceMap 20-Map 29User-designated data itemsSample TemperatureTempUser TemperatureTempTemperaturePPMS的温度计位置Neck ThermometerC
17、ernox/PlatinumThermometerOption ThermometerTempSys TempMap 20 Map 29Sample TemperatureSys TempBlock TempTemperaturePPMS的各种“Temperature”TempSample TemperatureSys TempDC_RACTMap 20 Map 29HCTTOACMSHorizontal RotatorHe-3 RefrigeratorTq-MagDC_RACTHCCernoxPlatinumCernox252323DC_RACT2727PPMS的各种“Temperature
18、”StandardHorizontal RotatorHe-3BaseSys TempRotator(User)TemperatureHe-3 TempDC_RSys TempUser Bridge Channel 1Channel 3ACTSys TempMap 23 System Bridge Channel 4Map 27HCMap 27(Sample Temperature)(Puck Temperature,Platform TemperatureMap 27TTOSys Temp(Sample Temperature)Hot:Map 21(Channel 1);Cold:Map 2
19、2(Channel 2)ACMSMap 25Tq-MagRotator(User)Temperature Map 23 Temperature从高温降温至10 K以下的操作Set Temperature 10.00K at 12.00K/min.Fast SettleWait For Temperature,Delay 120 secs,No ActionSet Temperature 1.80K at 1.00K/min.Fast SettleWait For Temperature,Delay 0 secs,No Action温度高于100 K时，先降温至10 K 15 K在10 K 15
20、 K停留一段时间，再降温！Commands:ChamberImmediate Mode and Sequence Mode样品室ChamberChamber Atmosphere样品室压强液氦液面指 示含 义Purging正在抽气Purged抽气结束，已封闭Sealed已封闭Vented充气结束，已封闭Venting正在充气Pumping持续抽气Flooding持续充气Pre-Hi Vac高真空预抽气At HiVac处于高真空Failure样品室操作故障HiVac Error 高真空故障Chamber温度 300 K磁场 1.0 TChamber AtmosphereDewarPumpCham
21、berVentValveFlushValveHe GasFlush ValveVent ValveSeal只是关闭Purge/Seal开关3次，最后关Vent/Seal关先开后关Pump Cont.开关Vent Cont.关开HiVac预抽开关Chamber温度低于295 K时不要执行Purge/Seal！Commands:MotionImmediate Mode and Sequence Mode步进马达水平旋转台MotionMotor:Stepper&ServoHorizontal Rotator:Stepper Motor ACMS：Servo Motor(伺服马达)PositionMo
22、ve toLocationSpeedPositionMove toIndexL角 度长 度磁场样品MotorMotion Control-8.512马达状态马达位置最大角度马达转动状态指示设定位置重新定义当前位置321MotionInstall Horizontal Rotator HardwareRemove Horizontal Rotator Hardware1.运行PPMS Tools中的MonQD6000.EXE2.在Send to PPMS菜单中点击Send Config3.选择C:QdppmsHorizontal RotatorConfig中的相应设置文件DC_R/Tq-Mag:
23、ACT/HRHR136.CFGHRACT136.CFG2.Send GPIB CommandsUSERTEMP 0.1.MonQD6000.EXE1.Utilities关闭温度计！HRPPMS的术语图解Field:Linear,No Overshoot,Oscillate,Sweep测量开始OscillateFast SettleNo OshootLinearPauseSweep时间温度磁场角度设定点Temperature:No Overshoot,Fast Settle,SweepStepper Motor:Pause,SweepMultiVuCommands:Bridge Channels
24、BridgePPMS Data Files PPMS Log Data Filev PPMS Configuration FilevUpload Data FilevHelium Data File Raw Measurement Data File Measurement Data FileData&FilesPPMS Log Data Filev用于PPMS诊断Data&Files时间系统状态磁体控制温度控制压强控制流量控制各种驱动器状态PPMS选件温度、电流等Advanced ItemsRaw Measurement Data Filev用于Measurement诊断v不同的选件会有不同
25、的格式v文件的大小：可能很大v必要性：一般不需要Data&FilesMeasurement Data Filev数据格式取决于所用的PPMS选件Data&FilesDC_RACTTq-MagACMSHC无自选数据TTO无自选数据Measurement Data Filev数据需要转换为按列的形式Data&FilesHeader;Copyright 1997-99,Quantum Design,Inc.All rights reserved.FILEOPENTIME,13199968.28,6/3/2003,9:38 AMBYAPP,LogData,1.0,2.0INFO,APPNAME,PPM
26、S MultiVu Application,Release 1.2.0 Build 5。DATATYPE,TIME,2DATATYPE,COMMENT,1DataComment,Time Stamp(sec),Status(code),Temperature(K),Magnetic Field(Oe),Sample Position(deg),Bridge 1 Resistance(ohms),Bridge 1 Excitation(uA),Bridge 2,13199968.36,4374,296.2498,-0.149,-8.512,-0.0049,-0.0147,48,0.00,0.00
27、,0.00,0.00,1.1262168,301.6772461,308.7025452,4374,300.000,-。HeaderData系统给出的检测数据Time Stamp(sec)Status(code)Temperature(K)Pressure()Map 25()System Status(code)Valve Position(deg)Plat Therm(K)13199968.364374296.24981.1262168301.6772461 437430.6296.249816913199973.314374295.93841.0962939301.6706543 4374
28、32.5295.938385013199978.314374295.53891.1105099301.6508484 437435.5295.538909913199983.384374295.21211.1105099301.6277466 437437.3295.2120972转换后的检测数据所有的数据处理软件都可以识别ExportData.exePPMS数据查看方式vGraph ViewvRecord ViewvTable ViewvRaw Data ViewData_ViewPPMS数据查看方式Data_ViewvGraph ViewvRecord ViewvTable ViewvRa
29、w Data ViewPPMS的数据与管理Data_ViewRecordTableRaw DataStatus Bar ToolbarSequence ControlSequence Command BarACMS Status LogOpenRestore GraphDefault GraphApply TemplateSave TemplateSave Template AsData SelectionAppearance Zoom PreviousAuto Scale All Plots+Graph ViewACMS Activated *.Dat：数据文件 *.Gph：图形文件 *.R
30、aw：原始过程数据*.Graph文件不是自动生成1、点击Data中的View；2、Graph菜单中打开*.DatTime Stamp&System StatusvTime Stamp(sec)：since midnight,January 1 of the current yearTime Stamp(sec)Status(code)Temperature(K)Pressure()13199968.36 4374 296.2498 1.126216813199973.31 4374 295.9384 1.0962939System Status(Code)System Controls：tem
31、perature,magnet,chamber,and sample positionJune 2,2003 at 18:39:28?Data_Time Stamp2003年6月3日 上午9:38?System Status(Code)Time Stamp(sec)Status(code)Temperature(K)Pressure()13199968.36 4374 296.2498 1.12621680 0 01 0 0 01 0 0 01 0110212=4096Sample PositionChamber PressureMagnetic FieldTemperature28=2562
32、4=1622=4Table A-2 in Appendix A:Data File Structures of PPMS Manual：Firmware Manualat target positionpurged and sealedstable/persistentnot validData_Status21=2PPMS Toolsv PPMS MultiVu Simulation PPMS 32-bit Toolsv HeGasMon32.EXEToolsPPMS 32-bit Toolsv桌面TOOLS文件夹中23个文件ToolsErrorLog.txtExportData.exeEX
33、PORTDATA.INIEyeSys.calfix1632lock.regGasmon32.exegauge.exeMagCalWizard.exeMagdiag2.exeMon6000.exeMon6500.exeMRCalWizard.iniMRCalWizard.pdfMRCalWizard.wscPPMSScript.incRemote32.exeRomcfg32.exeTable2d.exeTable2d.hlpTables.catTables32.EXETemp.engWizardState.incExportData.exeTools1.运行TOOLS中的ExportData.e
34、xe；2.确定原始数据文件和输出的数据文件；3.选择感兴趣的数据及其相对顺序；4.选择数据分隔方式（空格、制表位、逗号）；5.选择数据列的名字（Column Title）的格式；6.点击Export按钮。Gasmon32.exe1.用于监测系统温度_气体控制。2.不要关闭。Sequencev命令的关系：Sequence与ImmediateSequenceImmediateSequencePPMS MultiVu&Model 6000Sequencev界面的关系：Immediate与SequenceSequence_Immediate有无Sequence的组成SequenceHC Measure
35、mentLogPpmsData通用命令专用命令System CommandsAdvanced CommandsLogPpmsDataMeasurement Commands几个命令vWaitvScan TimevShutdownvMagnet ResetSequenceUniform mode 等间隔ln(t)mode对数间隔No Action等待Shutdown关闭温控Abort停止程序程序举例：磁性测量SequenceScan Temp from 5.0K to 300.0K at 12.0K/min,in 60 steps,Uniform,Fast Scan Field from 0.0
36、Oe to 10000.0Oe at 42.6Oe/sec,in 6 steps,Uniform,Linear,Persistent DC Mag 5 Scans Stickyrange Flags=33554439 AC Mag 100,1000,10000 Hz 2 Oe 1 Sec Stickyrange Flags=33554439 End ScanEnd ScanSet Field 0.0Oe at 42.6Oe/sec,Linear,PersistentShutdownEnd Sequence5 K 0.0 Oe DC Extraction AC Magnetization 200
37、0.0 Oe DC Extraction AC Magnetizaiton 10 K 0.0 Oe Bit FlagsDC Mag 5 Scans Stickyrange Flags=33554439Decimal Number0000 0010 0000 0000 0000 0000 0000 0111Binary NumberMap 31 Map 20225=33554432FieldTemperatureGeneral System StatusTable A-1 in Appendix A:Data File Structures of PPMS Manual：Firmware Man
38、ualMap 25PPMS程序的运行控制SequenceSequence RunSequence IdleSeq:Name.seqSeq:No.:Set Run正在运行Pause暂停运行Abort中断程序Lock锁定当前状态Lock SequenceLocked by:Zhao lOther Information:wait for me backLockCancel测量程序与数据文件的位置 C:My Documents Data Files Group 201 John Smith SequencesFile LocationGroup 202Group 203Group 204Group
39、205把程序文件和数据文件放在自己的子目录中。关于PPMS14H的选件PPMS Options根据所使用的选件不同完成下列步骤：1.连接相应的信号采集线（Cable)Connection Diagrams 2.启动相应的选件控制软件 Activate Option 3.根据选件安放样品选件及其控制软件见相应单元OptionActivate OptionActivateConfigure OptionLog PPMS DataUploadSend GPIB CommandsMagnet Error HandlingEvent LogHelium FillAvailable Options:Act
40、ive Options:Option ManagerAC TransportACMSHeat CapacityHelium3Low FieldResistivityThermal TransportTorque MagnetometerActivate-0Q 0T 0样品温升曲线热容量T tTt123系统温度漂移P=P0P=0电加热：Q=P0 t样品温升曲线的差异来源热容量加热器温度计加热器温度计样品的热扩散率 a样品与加热器和温度计的相对位置样品与加热器和温度计之间的热阻PPMS Heat Capacity热容量温度磁场压强热容量晶格比热高温：Dulong-Petit Law低温：T3 La
41、w中间温度：Debyes T3-LawT 0T 1T 2T 3 Einstein近似，电子比热表面PPMS HC的原理HC原理The Quantum Design Heat Capacity option measures the heat capacity at constant pressurePhysical Property Measurement System Heat Capacity Option Users Manual（Part Number 1085-150G）The Quantum Design Heat Capacity option controls the heat
42、 added to and removed from a sample while monitoring the resulting change in temperatureChapter 1PPMS HC的测量原理HC原理样品台Relaxation techniquePPMS HC的原理HC原理During a measurement,a known amount of heat is applied at constant power for a fixed time,and then this heating period is followed by a cooling period
43、 of the same duration.Small wires provide the electrical connection to the platform heater and platform thermometer and also provide the thermal connection and structural support for the platform.Chapter 1Relaxation techniquePPMS HC Thermal ModelsvSimple ModelHC原理Ctotal：样品及样品台（Platform）的热容量 T：样品台（样品
44、）的温度 Kw：引线的热传导系数 Tb：样品架（Thermal bath,均热块）的温度 P(t)：加热器的电功率。加热时为P0，冷却时为0PPMS HC Thermal ModelsvSimple ModelHC原理Tt降温：e-t/PlatformSample热接触良好PPMS HC Thermal ModelsvTwo-Tau ModelTMHC原理Cplatform：样品台（Platform）的热容量 Tp：样品台（样品）的温度 Kg：样品与样品台之间的热传导系数 Ts：样品的温度（拟合值）Csample：样品（Platform）的热容量热接触不良PPMS HC Thermal Mod
45、elsvTwo-Tau ModelTMHC原理样品与样品台之间的热接触PlatformSampleTypical Values of 1 and 2Cu RibbonPPMS HC的硬件v绝热条件的实现HC硬件1、高真空低温泵 一般可以达到：1.2 102 Pa 2、温度均匀区Contact BaffleContact Baffle AssemblyHC硬件.使温度均匀 .10 K以下吸附He测量热容量时使用。样品架温度计定标时取下。CharcoalPPMS HC的硬件v热源与温度检测样品架（Puck）HC硬件1、加热器可控功率电阻加热器2、热传导已知的引线PlatformHeaterPlat
46、form ThermometerPuckThermometer热接触338327327PPMS HC的硬件v热源与温度检测设备HC硬件1、Heat Capacity DSP Card加热器控制2、Model 6000“P2-System Bridge”温度控制 温度：Map 27。一般来说为样品架温度。理想情况：Rear Panel of Model 6500样品温度样品台温度样品架温度系统温度PPMS HC的硬件v接线框图HC硬件StandardHC/Helium-3Model 6500Model 6500PPMS HC的硬件v样品安装样品架的分类HC硬件Standard Puck and
47、He-3 PuckStandardHelium-3PPMS HC的硬件v样品安装样品台固定工具HC硬件1、Sample Mounting StationStandardHelium-3PPMS HC的硬件vHe-3 RefrigeratorHC硬件PPMS HC的硬件v样品架取放工具HC硬件样品架校正工具PPMS HC的软件v启动 Heat Capacity OptionHC软件PPMS HC Software VersionPPMS HeatCapacity 2.5.6 Build 8PPMS HeatCapacity 2.7.1 Build 0LatestCompiledJuly 27,2
48、001HC_PPMS能够测量什么？期望参数PPMS的设定功能如何实现热容量温度唯一设定的功能使用HC的软件热容量磁场恒定磁场：有使用HC的软件变化磁场：无Scan field相变潜热无此功能使用*.raw文件绝对温升无此功能使用DC_RPPMS HC的软件v功能介绍HC软件1.样品安装2.样品测量3.数据文件管理4.样品架定标5.背景文件的管理HC样品架的定标1.标定零磁场时的温度计、加热器的电阻样品架定标电阻温度关系Puck 327.calPuck 338-1.cal为什么？HC样品架的定标2.标定某一磁场时的温度计的电阻样品架定标温度计的电阻温度磁场关系Puck 327.calPuck 3
49、38-1.cal负磁致电阻效应样品架定标HC样品架的定标2.标定某一磁场时的温度计的电阻Puck 327.calHC的测量过程1.常用术语样品热容量Total HCAddenda HCSample HCPlatform Temperature(measured)实测样品台温度Platform Temperature(fit)模型拟合样品台温度Sample Temp(from fit)模型拟合样品温度Base Sample Temp加热前样品初始温度。一般和设定温度(Set point Temp)相同Averaged Sample Temp（始末温度平均）AddendaAvg Platform
50、TempSampleAvg Sample TempTwo-tauAvg Platform Temp Avg Sample TempHC的测量过程2.常用术语样品热容量Addenda：附加物 PlatformN/H GreaseSampleAddendaPPMS HC的测量过程样品热容量标定样品架的温度计和加热器测量附加物（Addenda）的热容量测量样品的热容量N Grease的热容量温度关系样品热容量Bunting,et al,Cryogenics,Oct.1969,pp.385-386热容量与磁场关系的测量vPlatform（氧化铝）的热容量与磁场的关系样品热容量HCT0Schottky