Characterization of fused cast refractories regarding their glass defect formation behaviour

Michael Dunkl Dr. M. Dunkl Consulting, Dsseldorf, Germany Jean-Piere Meynckens AGC, Belgium Janusz Zborowski AGH, University of Science and Technology
Cracow, Poland

23rd International Congress on Glass, Prague, 2013

Characterisation of fused cast refractories regarding their glass defect formation behaviour

Outline
1. Introduction

Characterisation of fused cast refractories regarding their glass defect formation behaviour

Outline
1. Introduction

2. Test methods
evaluating glass defect formation potential of refractories
2.1 2.2 2.3 2.4 Corrosion test Cords formation test Blistering test Exudation test

Characterisation of fused cast refractories regarding their glass defect formation behaviour

Outline
1. Introduction

2. Test methods
evaluating glass defect formation potential of refractories
2.1 2.2 2.3 2.4 Corrosion test Cords formation test Blistering test Exudation test

3. Conclusions

Introduction

Interrelations in glass defect formation process

properties of glass melt parameters of interaction between glass melt and refractory flow parameters properties of refractory

corrosion
parameters of melting process
construction of melting unit

glass defects

glass quality

Test methods

Corrosion tests
Static plate corrosion test as recommended by TC11 of ICG Experimental procedure

Pt/Rh-crucible 140 mm Quarzalcrucible

240 h / 1650 C

RT

Test methods

Corrosion tests
Static plate corrosion test as recommended by TC11 of ICG Experimental procedure

Pt/Rh-crucible 140 mm Quarzalcrucible

240 h / 1650 C

RT

What kind of information regarding glass defect formation potential we can expect from corrosion test ? (1)
Microstructure of reaction layer: FC AZS/borosilicate glass
after static plate corrosion test

thickness

100 m 100 m

What kind of information regarding glass defect formation potential we can expect from corrosion test ? (2)

Test methods

Modified static plate corrosion test

Additional possibilities of evaluation: qualitative assessment of glass defect formation potential, microscopic and EDX analysis of defects
10

Test methods

Cord formation test

Crucible test: - temperature change (e. g. 1550 1000 - 1550C) enhancing the formation of all kinds of defects (cords, stones, blisters) - evaluation of the polished plate cut from middle of the crucible

11

Test methods

Blistering test
with glass melt refreshing and continuous observation
miror lamp

video camera

refractory crucible
heating element

12

Test methods

Blistering test
comparison of blistering behaviour
Dynamic blistering test: AZS and HZFC with borosilicate glass at 1500C Blistering rate
20
Blistering rate [1/cmh], 6h-value

ZB-X950 HZFC
15
AZS ER 1711

10

0 0 48 96 144 192 240 288 336 384

test time [h]

13

Test methods

Exudation test
Method sample shape
cylinder

sample dimensions

procedure

evaluation/ remarks

ASTM C1223-92 A B

bar

disc

TC 11

bar

1 inch (diameter) 1 heating cycle 4 inch (hight) 4h soaking at 1510 C, 2 further cycles 1 x 1 x 4 inch possible 1 heating cycle 30 mm (diameter) 16 h soaking 30 mm (hight) at 1500 C 1 heating cycle 25 mm (diameter) 16 h soaking 3 mm (hight) at 1500 C up to 10 heating cycles 1st cycle 72h soaking further cycles 2h soaking at 50 x 50 x 100 mm 1550/1650C

calculation of sample's volume change calculation of sample's volume change calculation of sample's volume change determination of volume/weight of adhering glassy phase

14

Test methods

Sample

Method A "Glass Exudation" [%]

1 cycle 1500 C

TC 11 method

1550C
1 cycle 9 cycles

1650C
1 cycle 6 cycles

AZS 36
reduced exudation

AZS 41 AZS 32

1,1 - 1,6 0,9 - 1,8 1,0 -1,8

1,2 0,7 - 2,0 0,7 - 3,0

3,1 1,8 - 4,8 6,8 - 8,3

4,5 - 6,7 6,3 - 7,1 4,9 - 7,4 7,8 8,5 - 11 9,8 - 11,6

15

Test methods: Exudation test

results interpretation/meaning

(Some) Fundamental

statements

concerning testing and the results interpretation of lab exudation test

carried out on as delivered materials under air atmosphere 1. Sampling representativity and test method/conditions comparabilty

have to be ensured
2. lower amount of glass phase in FC AZS less exuded glass phase 3. lower exudation because 4. exudation test is not a corrosion test lower defect potential

Test methods

Conclusions
1. Standard and modified corrosion tests as well as cords formation tests combined with additional macro- and microscopic investigations are able to provide a valuable assesment of glass defect potential of a refractory/glass melt system To estimate the glass defect potential of FC refractories associated with their exudation behaviour properly it have to be kept in mind that: - what we determine in lab in the exudation test is not directly transferable on behaviour in a glass tank (corrosion process), - to evaluate and to compare the exudation data the sampling and test method parameters have to be known in detail and comparable
17

2.

Thank you for your attention

18