Norecs ProboStat Starting Manual Download Page 1

 

Complementary Material to ProboStat™ Manual

                                                

 

 

 

ProboStat™ Starting Guide 

As we are always learning from feedback from our customers and users, and for giving better understanding of 
the ProboStat™ sample holder, we present this note as a complementary material to the ProboStat™ Manual. 
The main goal of this document is explanation of the ProboStat™ system design which is not covered in the 
Manual.  

 

1.

 

ProboStat™ Gas Supply System 

 

1.1.

 

Recommended  reading 

First, we recommend familiarizing youself with: 

a)

 

ProboStat™ Manual: 

 

 

Part 2 “Safety first”, pp. 2-1 – 2-2, 

 

Part 4.2.4 “Gas connects”, pp. 4-5 – 4-7, 

 

Part 4.4 “Support tubes”, pp. 4-12 – 4.13, 

 

Part 4.5 “Gas supply tubes”, pp. 4-13 – 4-14, 

 

Part 6.3 “Pressures, vacuum, leakage rates, atmosphere purity”, pp. 6-1 – 6-2, 

 

Part 7.3 “Gas tightness”, pp. 7-4 – 7-5, 

 

Part 9.3 “Over-atmospheric pressure”, pp. 9-3 – 9-4, 

 

Part 9.4 “Wet gases with dew-point above room temperature”, p. 9-4, 

 

Part 12.1.4 “Inner gas tubes”, pp. 12-4 – 12-6. 

 

b)

 

NorECs web page www.norecs.com 

 

 

FAQ – atmosphere control  

 

FAQ – sealing 

 

1.2.

 

Single and dual atmosphere modes 

The ProboStat™ is a sample holder designed to perform experiments in single or dual atmosphere modes 
at near-atmospheric total pressure, and can be fed with virtually any gas. 

1.2.1.

 

Single atmosphere mode

 

The term “single atmosphere mode” means that one gas is fed in both inner and outer ProboStat™ gas 
compartments. The single atmosphere mode is used for: 

Summary of Contents for ProboStat

Page 1: ...rt 4 4 Support tubes pp 4 12 4 13 Part 4 5 Gas supply tubes pp 4 13 4 14 Part 6 3 Pressures vacuum leakage rates atmosphere purity pp 6 1 6 2 Part 7 3 Gas tightness pp 7 4 7 5 Part 9 3 Over atmospheric pressure pp 9 3 9 4 Part 9 4 Wet gases with dew point above room temperature p 9 4 Part 12 1 4 Inner gas tubes pp 12 4 12 6 b NorECs web page www norecs com FAQ atmosphere control FAQ sealing 1 2 Si...

Page 2: ...connects stems and stubs 1 3 1 Gas connects The gas connects mounted on the base unit hexagon are by default Swagelok quick connects In the high temperature base units the quick connects are replaced by Swagelok bulkheads and mounted on the top part of the splitted hexagon The stainless steel SS base unit has SS gas lines and SS quick connects steel colour The Ni coated brass base unit has copper ...

Page 3: ...aterial must be suitable for the gas used and softer material than the ferrules of the stem Fig 4 Brass quick connect stem with valve for IN s Fig 5 Brass quick connect stem without valve for OUT s The valve on the stems opens only when plugged to a quick connect with valve To plug or unplug a stem pull push it into the quick connect while holding back the rasterized collar We recommend having som...

Page 4: ... are extended to the high temperature zone by various gas supply tubes mounted on the base unit using gas stubs and piece of silicone hose The gas stub for the inner gas compartment is made of PEEK and assembled by a Viton sealing O ring The PEEK gas stub is screwed onto the upper part of base unit body The gas stub for the outer gas compartment is made of SS and assembled by two Viton sealing O r...

Page 5: ...w Table 3 Standard ProboStat O rings Size mm Amount pcs Material Mounting place Use Outer diameter thickness 40 3 1 Viton Isolast Alumina quartz or transport outer tubes Outer tube mounting Sealing the base unit outer gas compartment against environment Base unit protection during transportation 15 6 1 78 1 Viton Isolast Upper part of base unit body Sealing between inner and outer gas compartments...

Page 6: ... Straight 4 480 10 20 outer 1600 Alumina Straight 3 480 24 outer 1600 Quartz Bent 4 525 10 20 outer 950 Quartz Bent 3 525 24 outer 950 Alumina Multi bore 8 5 446 20 24 inner 1600 Alumina Straight 4 470 15 16 inner 1600 Alumina Straight 3 470 10 12 inner 1600 All numbers are for the system with 60 cm outer tube 1 6 Setting up gas compartments This part presents a step by step description how to cre...

Page 7: ...t Manual 8 Table 5 Assembling ProboStat gas compartments Step 1 Place the ProboStat base unit on the bench preferably fix it in a lab stand using a bar for base unit fixture Step 2 Mount the inner gas supply tube onto the PEEK gas stub ...

Page 8: ...al 9 Step 3 Mount the sample support tube tight Step 4 Place an Au sealing ring on top of the sample support tube This step is relevant for the gas compartments separation If you plan to measure using the single atmosphere mode skip this step ...

Page 9: ...ep 5 Place a sample on top of the gold ring or directly on the sample support tube for the single atmosphere mode Check that the gold ring and sample are centered Step 6 Mount outer bent silica a or straight alumina b gas tube onto the SS gas stub a ...

Page 10: ...nt silica a or straight alumina b gas tube onto the SS gas stub Step 7 Mount enclosing quartz or alumina tube and O ring For simplicity the spring load assembly is not explained or drawn here In real setup it is always present and push the sample down on the AU ring b ...

Page 11: ...Complementary Material to ProboStat Manual 12 Step 8 Fasten the base unit flange ...

Page 12: ...e contact 2 2 Electrode contact assemblies Electrode contact assemblies hereafter called electrode contacts are assigned to contact the ProboStat base unit with a test sample located in the high temperature zone 2 2 1 Description and denotation The electrode contacts for electrical measurements come in variety of types Many of them are issued in 2 wire pairs one for current and one for voltage Tab...

Page 13: ...Complementary Material to ProboStat Manual 14 Tabel 7 ProboStat electrode contacts Electrode contact drawing Code H2N INH2N12 IN2 ...

Page 14: ...Complementary Material to ProboStat Manual 15 Electrode contact drawing Code GR GP2 GP1 ...

Page 15: ...Complementary Material to ProboStat Manual 16 Electrode contact drawing Code H1TN10 H1BN10 vdP2 ...

Page 16: ...gger mini contacts 2 2 3 Mini contacts Supplied electrode contacts and thermocouples see below are soldered to female mini contacts matching to the base unit feedthroughs The mini contacts are made of Au and Ni plated brass and have size 22AWG HV version 20AWG 2 2 4 Soldering of mini contacts When soldering insert an appropriate metal wire into the mini contact and add solder by tiny portions unti...

Page 17: ...bering and standard material of the electrical wiring for the base unit feedthroughs top view in relation to the gas inlets I and outlets O Also the Phoenix type chassis multi connector that was fitted to early version is shown The coding and functions are listed in detail in the table below We strongly recommend users to print the Wiring Overview page 14 2 or 14 3 in the ProboStat manual and hang...

Page 18: ... 4 G Pt Inner low voltage ILV c ILV 5 G Pt Low current shield LCS i j LCS 6 G Pt Low current Guard LC b LC 7 G Pt Low voltage shield LVS k l LVS 8 G Pt Low voltage LV d LV 9 P Green NiCr Top TC TCT TCT 10 N White NiAl Top TC TCT TCT 11 P Green NiCr Centre control TC TCC TCC 12 N White NiAl Centre control TC TCC TCC 13 G Pt High voltage HV g HV 14 G Pt High voltage shield HVS o HVS 15 G Pt High cur...

Page 19: ... the base unit hexagon The electrical feedthrough consists of male mini contact sitting in PEEK insulator and soldered to compensation wire The feedthroughs are numbered starting with very top of the base unit and run clockwise from 1 to 4 The numbering continues on the outer ring from 5 to 16 again clockwise The feedthroughs no 1 4 are located in the inner gas compartment no 5 16 in the outer Fig...

Page 20: ...tive Green NiCr K type thermocouple positive 2 3 5 Signal and shield feedthroughs The ProboStat base unit has 10 electrical feedthroughs 6 of them lead current or voltage signal 4 shield The signal feedthroughs are soldered to the center of the BNC contacts shields to the plates ILC and ILV feedthroughs do not have own shield feedthroughs However shield is important for some measurement instrument...

Page 21: ...th ends for convenient use These color marks have nothing to do with any codes or denotation on the ProboStat or measurement instruments Fig 16 A coaxial cable with color mark 3 ProboStat temperature control system In this part we describe ProboStat thermocouple assemblies and base unit thermocouple wiring 3 1 Recommended reading We recommend familiarizing youself with a ProboStat Manual Part 4 7 ...

Page 22: ...ariety of types listed in the Tables 9 10 Table 9 Thermocouples denotation Code Type X Description TCT D X S K Disk sample top thermocouple assembly TCI D X S K Disk sample inner thermocouple assembly TCC D X S K Disk sample control thermocouple assembly TCC B X S K Bar sample control thermocouple assembly TCB B X S K Bottom thermocouple assembly for Seebeck coefficient measurements TCT B X S K To...

Page 23: ...Complementary Material to ProboStat Manual 24 Table 10 ProboStat S type thermocouple assemblies Thermocouple drawing Code TCC D TCC B TCT B TCB B ...

Page 24: ...re negative pole the black wire positive The K type thermocouple marked with white and green the white wire negative pole the green wire positive Fig 17 Thermocouples color codes S type black and red K type green and white 3 4 ProboStat thermocouple wiring Three thermocouples can be connected to the ProboStat base unit one in the inner gas compartments and two from the outer one see the Wiring ove...

Page 25: ...S type base unit have orange color mounted on the K type base unit green Fig 19 Thermocouple sockets for S type base unit Fig 20 Thermocouple sockets for K type base unit 3 5 Mounting thermocouples on the base unit Depending on measurement method one of three thermocouples should be mounted onto the base unit Three thermocouples are needed for the Seebeck coefficient measurements only When mountin...

Page 26: ...hermocouple The furnace and the ProboStat thermocouples are located at different positions resulting in a temperature gradient This gradient can be as high as 20 30 degrees 4 ProboStat spring load assemblies The ProboStat can be equipped with two different spring load assemblies for different purposes triangular top plate spring load assembly and two rod van der Pauw spring load assembly 4 1 Recom...

Page 27: ...g load assembly is used in all measurement setups except van der Pauw The triangular top plate spring load assembly consists of a top plate three long alumina bars with Pt locks and three springs Fig 22 The triangular top plate spring load assembly parts 4 3 Two bars van der Pauw spring load assembly A two bars van der Pauw spring load assembly is used to press the four electrodes of van der Pauw ...

Page 28: ...s in the triangle top plate Hook springs over the base unit pedestal Fig 23 Mounted spring load assembly High temperature part of ACIS setup Fig 24 Connections to the ProboStat base unit 4 4 2 Two bars van der Pauw spring load assembly In order to use this assembly you need four electrode contacts Please see the ProboStat manual Fig 25 Top part of van der Pauw setup The spring load assembly is mar...

Page 29: ...roboStat water cooling system We recommend familiarizing youself with the ProboStat Manual Part 4 2 2 Water cooling pp 4 3 4 4 Part 4 2 3 Connector box and cooling water ring change angle of the fixation bar pp 4 4 4 5 Cooling water hose can be connected to the ProboStat base unit via two stubs on a water cooling cylinder The water flows between the water cooling cylinder and the central base unit...

Page 30: ...ng water hose stubs on water cooling cylinder Fig 28 Water cooling O rings Fig 29 Cooling water connected 6 ProboStat Earth On the base unit hexagon you can you can also find Earth point screw that is used for external Earth connection Fig 30 Earth point screw ...

Page 31: ...ider only one example to cover the most common questions Let us consider 2 point impedance spectroscopy and conductivity measurements on disk sample as an example See the ProboStat manual part 8 2 2 pp 8 2 8 7 7 1 Assembling 2 point impedance spectroscopy and conductivity measurements on disk sample 7 1 1 List of accessories In order to find out all parts you need for this method you should refer ...

Page 32: ...C and LV The second electrode contact is connected to the feedthroughs no 13 and 15 HV and HC The optional inner thermocouple should be connected to the feedthroughs no 1 and 2 TCB There are two equivalent ways for the thermocouple connection The thermocouple can be connected to the feedthroughs no 9 and 10 TCT or 11 and 12 TCC 7 1 3 Cable connections The cable connections depends on the electrode...

Reviews: