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燃料電池測試系統/高溫固定裝置
ProboStat, overview

【Norecs】高溫電氣測量系統和週邊設備 ProboStat™ 系統

燃料電池測試系統/高溫固定裝置

簡介

ProboStat™

裝置通過適用於標準阻抗譜儀連接器的同軸電線和標準熱電偶補償電線進行電氣連接。 氣體可以通過單腔或雙腔模式被直接輸入或通過電極輸入,從而可以在受控氣氛下進行測量,以梯度方式測量傳輸數並測試燃料電池,泵和感測器元件。 氣體通過Swagelok快速接頭供應。

我要諮詢

ProboStat燃料電池測試系統概述

被測樣品放在大約一個 50 cm長的氧化鋁支撐管上,位於封閉的氧化鋁或二氧化矽外管內。 樣品可以與2個,3個或4個電極接觸(例如鉑金,可以使用圓盤,范德堡( van der Pauw) 或條形製作)。 一個氧化鋁彈簧元件將樣品和電極固定在適當的位置。 16個電氣饋通允許使用4條遮罩電極引線,表面保護層和多達3個熱電偶(例如用於Seebeck係數測量)。 裝置通過適用於標準阻抗譜儀連接器的同軸電線和標準熱電偶補償電線進行電氣連接。 氣體可以通過單腔或雙腔模式被直接輸入或通過電極輸入,從而可以在受控氣氛下進行測量,以梯度方式測量傳輸數並測試燃料電池,泵和感測器元件。 氣體通過Swagelok快速接頭供應。

被測材料性能及適用方法:

  • 電導率與T,pO2,pH2O等的關係
  • 直流,交流,阻抗譜
  • 介電性能,損耗..等
  • 圓盤狀,范德堡和條狀
  • 2、3和4個電極
  • 離子遷移數
  • 質子遷移數
  • H / D同位素效應
  • 塞貝克係數
  • I-V特性
  • 燃料電池元件和單電池測試
  • 電極動力學
  • 出口處的電化學泵送,氣體滲透和電催化以及氣體分析(例如GC或MS)
  • 感測器測試
  • 高壓(kV)版本可以進行鐵電體的極化
  • 大電流版本
  • 受控氣氛下的退火或燒結

下圖為連接盤裝樣品進行阻抗測量的示例。 原理圖顯示了彈簧的使用原理以及帶有雙氣源和熱電偶的常規2電極4線設置。 下面圖片顯示了帶有饋通的基座的一部分

ProboStat燃料電池測試系統說明

用於在高溫和受控氣氛中進行電氣特性等:

  • 室溫-1600°C
  • 幾乎適用於任何氣體(單或雙)
  • 盤狀樣品(10-24mm)或條狀樣品

裝置由一個基座組成,該基座具有16個電氣饋通孔,4個氣體饋通孔,樣品支撐管固定裝置,外管,彈簧和冷卻水。
各種幾何形狀的樣品放置在支撐管上,通過各種電極進行連接,並通過陶瓷彈簧固定在適當的位置。 附加設備通常包括帶電源和控制器的管式爐,電氣特性裝置(阻抗譜儀,電壓表,恆電位儀等)和氣氛控制裝置(例如氣體混合器)。

 

多功能性

  • 一個裝置; 多種配件,方法和可能性:
  • 電導率與T,pO2,pH2O等的關係
  • 直流,交流,阻抗譜
  • 介電性能,損耗等
  • 圓盤狀,范德堡和條狀
  • 2、3和4個電極
  • 離子遷移數
  • 塞貝克係數
  • I-V特性; 燃料電池元件和單電池測試
  • 電極動力學
  • H / D同位素效應
  • 出口處的電化學泵送,氣體滲透等
  • 感測器測試     

封閉管內部視圖:支撐管,樣品(隱藏),電極連接,彈簧和供氣管與高溫爐一起使用的典型配套設置

ProboStat測量設備可與所有阻抗分析儀,恒電位儀和萬用電錶一起使用。 我們的理念是保持其相容性,併為使用者配備可更換的部件(使用者也可自行製造),以實現長久的使用壽命和長期的經濟效益。

ProboStat配件及可替換部分:

  • 標準裝備:TC,電極接點等
  • 用於樣品或粉末退火的坩埚架配件
  • 不鏽鋼基座,用於腐蝕性氣體
  • 不鏽鋼外管,用於遮罩或高壓情況
  • 用於極化,擊穿等目的的高壓(kV)版本
  • 液體電介質的液體電池
  • 用於熔鹽融化的固態電池
 

基座是ProboStat系統的主要部分; 所有版本均與所有附件和方法相容(kV版本除外)

樣品:

我們可以用特定材料製造具有或沒有電極以及PLD靶的燒結樣品。 我們還可以提供適合ProboStat尺寸的某些第三方樣品(例如SOFC紐扣電池)。

高溫爐及加熱罩:

我們還提供與ProboStat配套使用的高溫爐及加熱罩。

ProboStat燃料電池測試系統裝配

根據應用方法和條件的變化,ProboStat高溫測量裝置可以用多種不同配件進行組裝。 裝置的所有零部件都是可拆卸並替換的,這些零部件可以從NORECS購買,使用者也可以根據自身需要自製。 

圖所展示的是一套常規配置的ProboStat裝置,用戶根據需求可自行更改配件類型及數量。

通常,所含零部件包括:

(1)外部封閉管:可選材質包括氧化鋁,石英以及鋼管。

(2)樣品支撐管(以氧化鋁為準):

  • 盤狀樣品 (管徑10-24mm)
  • 條狀樣品
  • 特殊類型 (液態電池,遮罩管,坩埚架,YSZ, 其他材料等)

(3)電極接點和熱電偶(以氧化鋁和鉑為準):

  • GP#用於可更換的電極套(4點條狀樣品)或GP2N電極接點。
  • H#直接接觸圓盤上的電極或條狀樣品的末端電極。
  • GR#用作圓盤樣品的參考電極或保護環。
  • IN2用於從支撐管內部接觸磁碟樣品上的下端電極,從而允許在其周圍使用參比電極或保護電極,或將盤狀樣品密封到支撐管上用於濃縮電池,燃料電池或其他電化學電池的實驗。
  • VDP2成對使用,用於van der Pauw測量。
  • TC是用於各種用途的熱電偶。
彈簧:
  • 20mm和24mm版本用於所述或更小直徑的樣品。
  • 替換品及備用件。
  • 彈簧(軟,硬)
燃氣管
  • 直管,氧化鋁。
  • 彎管,石英。
  • 矽膠軟管,用於裝置腔內連結。
小零件:
  • 金或銀質環形墊圈,氧化鋁熱電偶蓋,氧化鋁樣品支撐板,氧化鋁墊片環,備品。

外部連接:

  • Swagelok快速連接閥桿,用於進出氣體。
  • 用於阻抗分析儀等的BNC同軸電纜。
  • 熱電偶接點。
  • 冷卻水。

ProboStat燃料電池測試系統配套設備

ProboStat™高溫測量固定裝置既可以作為一台獨立設備進行寄送,也可與其他與材料研究有關的設備共同構成成套裝置一起寄送。 除ProboStat樣品架以外,這樣的成套裝置通常還包括以下設備:

高溫爐和控制器 NORECS 提供專為 ProboStat™ 樣品架改裝的商用爐和加熱罩,並配有控制器。
測量儀器 NORECS提供商業化的儀器,比如阻抗分析儀,恒電位儀,萬用表或多工器。
測量軟體 測量軟體—Omega包括並實現以下功能:
•控制並讀取品質流量控制器,減壓閥, 以及支援Modbus或GPIB協議的高溫爐和其他測量儀器。
•利用萬用表測量感測器和儀錶,以驗證電壓和電流和類比信號輸出。
•包括解釋讀取值(如熱電偶電壓)的函數。
•在螢幕上繪圖,並將所測得數據保存於硬碟上。
氣氛控制裝置 NORECS製造多種類型的氣體混合器,包括標準版本和客戶定製版本。 例如:
(1)ProGasMix FC — 基於多功能轉子流量計的手動氣體混合器,適用於:
•燃料電池實驗,需要對燃料和/或氧化劑加濕
•氣體滲透性測量
•遷移數測量
•電導率測量值與pO2, pH2O, pH2等的關係
(2)FCMix — 簡單的氣體混合器,用於小型燃料電池的加濕和超壓控制。

ProboStat™樣品架還可以隨附以下附件:

  • 應用於高壓,最高達15bars。
  • 高溫下液體的介電常數和電導率的測量。
  • 粉末在受控氣氛中的退火。
  • 塞貝克係數測量中創建溫度梯度。
  • 靠近樣品氧氣感測器的氧氣水平測量。

ProboStat燃料電池測試系統規格

  • 外管直徑:40mm
  • 全長:75cm,提供較短版本(-10,-20,-30cm)
  • 單側電池組裝
  • 樣品固定:通過氧化鋁棒的彈力
  • 所有熱區電極引線均可通過饋通微型連接器拆卸
  • 直徑為10至24mm的可拆卸支撐管系統
  • 適用於直徑最大為24 mm的盤狀
  • 適用於長度最大為50 mm的條形樣品
  • 溫度:長期:<1400ºC,短期:<1600ºC
  • 氣體環境:氧化,還原或腐蝕; 濕或干; 從小過壓到低真空
  • 6 BNC電極連接,用於阻抗分析儀..等
  • 內部遮罩橋接,接地和保護開關
  • 3個熱電偶連接
  • 4個Swagelok氣體快速連接到1/8''管道(可根據要求提供其他連接)
  • 標準材料:氧化鋁AL23,Pt,Pt10%Rh,鍍鎳黃銅
  • 可以對冷端基板進行水冷(或加熱)
  • 16個電氣穿通孔(4個內腔,12個外腔),額定100V,每個5A​

Brief description

The sample under test rests on a ca. 50 cm long support tube of alumina, inside a closed outer tube of alumina or silica. The sample can be contacted with 2, 3 or 4 electrodes of e.g. platinum, using disk, van der Pauw, or bar geometries. A spring-loaded alumina assembly holds the sample and electrodes in place. 16 electrical feedthroughs allow use of 4 shielded electrode leads, surface guard, and up to three thermocouples (e.g. for Seebeck coefficient measurements). Electrical connections are made via coax cables suitable for standard impedance spectrometer connectors, and standard thermocouple compensation cables. Gases can be fed in single or dual chamber modes directly onto or from electrodes, allowing measurements under controlled atmospheres, transport number measurements in gradients, and testing of fuel cell, pump, and sensor components. Gas supply is via Swagelok quick-connects.

Materials properties measured and applicable methods

  • Conductivity vs T, pO2, pH2O, etc.
  • DC, AC, impedance spectroscopy
  • Dielectric properties, loss, etc.
  • Disk, van der Pauw, and bar geometries
  • 2, 3, and 4 electrodes
  • Ionic transport number
  • Proton transport number
  • H/D isotope effects
  • Seebeck coefficient
  • I-V-characteristics
  • Fuel cell components and single cell testing
  • Electrode kinetics
  • Electrochemical pumping, gas permeation and electrocatalysis with gas analysis (e.g. GC or MS) on outlets
  • Sensor testing
  • Poling of ferroelectrics possible with the high-voltage (kV) version
  • High-current version
  • Annealing or sintering under controlled atmosphere

Example of connection to disk samples for impedance measurements. The schematics show principle of spring loads and regular 2-electrode 4-wire setup with dual gas supplies and thermocouple. Part of base unit with feedthroughs is shown in the photo below.


for electrical characterisation etc. at high temperatures and in controlled atmospheres.

  • RT-1600°C
  • Almost any atmosphere (single or dual)
  • Disk (10-24 mm) or bar samples

The cell consists of a base unit with 16 electrical feedthroughs, 4 gas feedthroughs, fixtures for sample support tube, outer tube, spring load, and cooling water.

Samples of various geometries rest on the support tube, is contacted via various electrode connects, and held in place with a ceramic spring load. Additional equipment usually comprise tube furnace with power supply and controller, electrical characterisation (impedance spectrometer, voltmeter, potentiostat, etc.) and atmosphere control unit (e.g. gas mixer).

One cell; many accessories, methods, properties:

  • Electrical conductivity vs T, pO2, pH2O, etc.
  • DC, AC, impedance spectroscopy
  • Dielectric properties, loss, etc.
  • Disk, van der Pauw, and bar geometries
  • 2, 3, and 4 electrodes
  • Ionic transport numbers
  • Seebeck coefficient
  • I-V; Fuel cell components and single cells
  • Electrode kinetics
  • H/D isotope effects
  • Electrochemical pumping, gas permeation, etc.
  • Sensor testing

Typical view Inside the enclosing tube: Support tube, sample (hidden), electrode connects, thermocouple, spring load, and gas supply tube.

The ProboStat measurement cell works with all impedance spectrometers, potentiostats, and multimeters.  Our philosophy is to keep it versatile and with user-replaceable parts (that the user can also manufacture) for good lifetime and long-term economy.

Accessories and options for ProboStat

  • Standard furnishment: TCs, electrode contacts, etc.
  • Crucible holder accessories for sample or powder annealing
  • Stainless Steel base unit option for corrosive gases
  • Stainless Steel outer tubes for shielding or high pressures
  • High voltage (kV) version for poling, breakdown, etc.
  • Liquid cell for dielectrics of liquids
  • Melting solid cell for molten salts 
 

The base unit is the main part of the ProboStat system; all versions compatible with all accessories and methods (except kV version).

Samples

We can manufacture sintered samples of selected materials, with or without electrodes. We may also provide certain third-party samples (e.g. SOFC button cells) suitable for ProboStat dimensions.

Power-supply and temperature controller

We re-sell or recommend furnaces or heating mantles for ProboStat from third-party manufacturers.

Furnaces and heating mantles

We re-sell or recommend furnaces or heating mantles for ProboStat from third-party manufacturers.

The ProboStat™ high temperature measurement cell can be furnished with a wide range of parts depending on the method and conditions. All parts are detachable and replaceable, and can be bought from us or manufactured by the user according to instructions and measures contained in the manual. The example packages contain typical selections of these parts, but other combinations are of course possible.

The options, furnishment and parts comprise:

(1)Outer enclosing tubes

  • Alumina, quartz, Steel

 (2)Sample support tubes (alumina standard)

  • Disk samples (tube diameters 10-24 mm)
  • Bar samples
  • Special versions (liquid cell, shielded tube, crucible holder, YSZ, other materials, etc.)

(3)Electrode contacts and thermocouples (alumina and Pt standard)

  • GP# are used for replaceable electrode wraps (4-point bar samples) or GP2N electrode contacts
  • H# make direct contact to electrodes on disks or end electrodes on bars
  • GR# are used as reference electrodes or guard rings on disk samples
  • IN2 is used to make contact to the lower electrode on a disk sample from inside the support tube, thus allowing the use of a reference or guard electrode around it, or sealing the disk to the support for concentration cell, fuel cell, or other electrochemical cell tests.
  • VDP2 are used pairwise for van der Pauw measurements.
  • TC's are thermocouples for various uses.

Spring loads

  • 20 mm and 24 mm versions for samples of said or smaller diameter.
  • Replacements and back-up sets
  • Springs (soft and hard)

Gas tubes

  • Straight, alumina
  • Bent, quartz
  • Silicone hose for in-chamber connections

Small parts

  • Gold or silver ring gaskets, alumina thermocouple caps, alumina sample support plates, alumina spacer rings, spares

External connections

  • Swagelok quick connect stems for gases in and out
  • BNC coaxial cables for impedance spectrometers etc.
  • Thermocouple contacts
  • Cooling water

 

Typical components in a setup for materials characterization with ProboStat™

The ProboStat™ measurement cell can be delivered as a single unit or as part of a complete setup for materials characterization. Such complete system contains, in addition to the  ProbStat™ sample holder, typically of the following components:

Furnace and controller NORECS offers commercial furnaces and heating mantles, with controller,specifically modified for the ProboStat™ sample holder.
Measurement instrumentation NORECS can supply commercial available instrumentation such as
impedance spectrometer, potentiostat, multimeter or multiplexer.
Software Our measurement software Omega includes and allows:
  • Control and read mass flow controllers, pressure regulators,furnaces and other measurement instruments with Modbus or GPIB protocol support.
  • Use multimeters to measure sensors and gauges to have analog voltage or current output.
  • Include functions to interpret the read values such as thermocouple voltage.
  • Plot on screen and save to disk the measured data.
Atmosphere control equipment

NORECS manufacture several gas mixers, both standard and customized.
Examples:

ProGasMix FC - Versatile rotameter-based manual gas mixer, suitable for

  • Fuel cell tests, with humidification of fuel and/or oxidant
  • Gas permeation measurements
  • Transport number measurements
  • Conductivity measurements as a function of pO2, pH2O, pH2, etc.

FCMix - simple gas mixer, humidification and overpressure control for small
fuel cells.

The ProboStat™ sample holder can in addition be delivered with accessories for:

  • Applying high pressures, up to max. 15 bars.
  • Measurements of dielectric constants and conductivity of liquids at high temperatures Liquid cell
  • Annealing of powders in controlled atmospheres
  • Creating temperature gradients in Seebeck coefficient measurements internal heater instructions
  • Measurements of oxygen level close to the sample oxygen sensors

Specifications

  • Outer tube diameter: 40 mm
  • Overall length: 75 cm, shorter versions available (-10, -20, -30 cm) 
  • Single end cell assembly
  • Sample fixation: spring force via alumina rods
  • All hot-zone electrode leads detachable via feedthrough mini-connectors
  • Support tube systems from 10 to 24 mm diameter detachable
  • For up to 24 mm diameter disk samples
  • For up to 50 mm long bar samples
  • Temperature: typical long term: < 1400ºC, short term: < 1600ºC
  • Atmosphere: Oxidizing, reducing, or corrosive; wet or dry; from small overpressure to low vacuum
  • 6 BNC electrode connections for impedance spectrometers etc.
  • Internal shields bridging, ground and guard switches
  • 3 thermocouple connections
  • 4 Swagelok gas quick-connects to 1/8'' tubing (other connections on request)
  • Standard materials: Alumina AL23, Pt, Pt10%Rh, Ni-plated brass
  • Water cooling (or heating) of cold end base unit is possible
  • Spare parts supply, also of hot zone consumables
  • 16 electric feedthroughs (4 inner chamber, 12 outer chamber). Rated for 100V, 5A each