Development of a TG/DTA Instrument with High-Resolution ... · Development of a TG/DTA Instrument with High-Resolution Sample Observation Capability and Some Applications Author:

Development of a TG/DTA systemwith high resolution optical observation capability

and its Advantages

08/12/2015

NATAS 2015

Brian Goolsby, Yoshikazu Nishiyama*, Masayuki Iwasa*, Kenichi Shibata*

Copyright ©2014 Hitachi High-Tech Science Corporation All Rights Reserved.

Introduction - The Problem

• In conventional TG/DTA instruments, samples cannot be viewed directly because they are obscured by the ceramic furnace, heating elements, insulation, etc.

• So, TG/DTA users are left to determine which phenomena occur by reviewing the TG and DTA curves obtained during the analysisduring the analysis.

Melting ?

Ｄ

Exo.Decomposition ?Evaporation ?

SampleIncrease

ＤＴＡ Endo.

Sample

FurnaceＴＧ

Decrease

Temperature


Temperature

Introduction – A Proposed Solution

• Almost all of these events could be confirmed visually

• A new TG/DTA design featuring a furnace structure that g gmakes sample observation possible.

• The new design should provide the same quality data output as the original instrument, while also providing additional useful information about the material flow, shape change, and even unexpected events.p g p

• This presentation highlights some examples of the optical observation TG/DTA system in action


Design Challenges

1. Is it possible to view the inside of the furnace during measurement while maintaining:

uniform heating- uniform heating- high sensitivity- controlled environment (gas

Heating elements, insulation

composition / flow rate)

C i f t bCeramic furnace tube

Fig.1 Structural features of a conventional horizontal TG/DTA

2. Can images be recorded in a really useful manner?To view a sample, equipment has to be installed near the furnace, which


can be challenging for a camera.

Study

-At last NATAS, we showed thermal analyzer data linked with optical images and its advantageswith optical images and its advantages .-However, currently the almost product and parts is going to be smaller than smaller, so there are need to see more d t il th l d t d l ti l idetail on thermal data and also optical images.

Approach for itTh l A l N d hi h iti it l d d-Thermal Analyzer: Need high sensitivity – already done-Optical Image: High resolution – Think about heat resistance


High resolutions camera mount on furnace

Mirror

Light

Light


Camera

High resolutions camera mount on furnace

Conventional design New design


Resolution Comparison on Wood material

Can zoom up with digital zoom


Advantage of high resolution camera on Wood

800

600

20.0

0 0

1400.0

1200 0 600

400

0.0

-20.0

40 0

°C

1200.0

1000.0

Ignition Point

DTA

/

V 200

0

TG

/ %

-40.0

-60.0

Tem

pera

ture

/

800.0

600.0

-200

-400

-80.0

-100.0

400.0

200.0

Time / min60.050.040.030.020.010.00.0

-600 -120.00.0


Advantage of high resolution camera on Wood

Conventional Camera

New camera

Please add comment


Application of milled Carbon


#1 #6


1.4

1.2

20.0

0.0

1600

1400

#1 #6/

mV

1.0

0.8

0 6 G/

%

120.0

-40.0

-60 0ture

/ °

C

1200

1000

800

#5

#6

#7

#2 #7

DTA

0.6

0.4

0.2

TG60.0

-80.0

-100.0

Tem

pera

t 800

600

400

#2#3#4 #8

#7

#3 #8

Time / min80.060.040.020.00.0

0.0

-0.2

-120.0

-140.0

200

0

#2

#1 #10#9

#4 #9

#5 #10*Carbonsample weight : 5mg

℃


heating ratepurge gas

: 10℃/min: Air 200mL/min


#3

#3 #5#5

Residue

Residue

#7#6 #10


Application of Coating material



#3 #8#1 #2 #3 #8#1 #2

#4 #9700

600

500

20.0

0.0

-20 0

#5 #10

TA

/

V

500

400

300

TG

/%

-20.0

-40.0

-60.0

#6 #11

D

200

100

0

-80.0

-100.0

-120.0

#2 #5#1 #3 #10

#8

#9#7

#11 #12

#7 #12Temperature / °C1000.0800.0600.0400.0200.0

-100 -140.0#4 #6

*Coating material


sample weightheating ratepurge gas

: 5mg: 10℃/min: Air 200mL/min


#8 #9#8

#12#10 #11

The black specks were in sample at #8-9. After decomposition around 600°C (#10) those were not there


decomposition around 600 C (#10), those were not there.

Summary

The TG/DTA with sample observation capability features:- A quartz furnace tube and a view port- Image recording is accomplished with a camera unit designed with heat resistance in mind.- Software allowing overlay of each image with the corresponding data

f G/Testing of various materials with the new TG/DTA design has demonstrated a number of benefits, including:- Data interpretation is easier when more information is available- More exact understanding of transitions can be gained- Changes in physical state, such as color, that may not have an

associated mass changeU t d f ki d t b l i d- Unexpected or one-of-a-kind events can be explained


END

Development of a TG/DTA systemwith high resolution optical observation capability

d it Ad tand its Advantages


Documents

Development of a TG/DTA Instrument with High-Resolution ... · Development of a TG/DTA Instrument with High-Resolution Sample Observation Capability and Some Applications Author: