mössbauer spectroscopic and chromaticity analysis on the colourative mechanism of ancient goryeo...

MÖSSBAUER SPECTROSCOPIC AND CHROMATICITYANALYSIS ON THE COLOURATIVE MECHANISM OF

ANCIENT GORYEO CELADON FROM GANGJIN AND BUAN*

A. Y. JEON, H. G. NO, U. S. KIM, W. S. CHO, K. J. KIM and J. Y. KIM†

Korea Institute of Ceramic Engineering and Technology, Icheon Branch, Gyeonggi-do 467-843, Korea

C. M. KIM and C. S. KIM

Department of Physics, Kookmin University, Seoul 136-702, Korea

and G. I. KANG

Gangjin Celadon Museum, Jeollanam-do 527-872, Korea

In ancient Goryeo celadon excavated from the kiln sites in the GangJin and Buan areas, theeffect of the chemical composition and ionic state of Fe on the colour was evaluated byMössbauer spectroscopy and chromaticity analysis. According to chromaticity analysis, the L*value (brightness) of the glaze was shown to be affected more by TiO2 and MnO than by Fe2O3,and the body was affected more by Fe2O3 than by TiO2. The a* value was found to be affectedby Fe2O3 and TiO2 in the glaze, whereas there was hardly any change in the body accordingto the composition. As for the b* value, changes due to the composition were shown to besmaller than those for the L* and a* values. According to the Mössbauer spectroscopy results,as the quantities of TiO2 and Fe2O3 are increased, Fe2+/Fe3+ decreases; while the changes inFe2+/Fe3+ with MnO and P2O5 are negligible. As the quantity of Fe2+/Fe3+ increases, the a* andb* values decrease, which results in the change of colour from red–yellow to blue–green. Thecharacteristic green colour can be attributed to increased L* (brightness) and decreased a*and b* values (blue–green shift) due to the reduced Fe ion, which is mainly determined by theTiO2 and Fe2O3 contents.

KEYWORDS: CELADON, PORCELAIN, MÖSSBAUER SPECTROSCOPY

INTRODUCTION

Goryeo celadon has been acknowledged for its artistry thanks to not only its plastic beauty, butalso the subtle green colour. Goryeo celadon is well known for its unique production methods,including inlay techniques, and as pottery with a beautiful colour, called the ‘celadon greencolour’. Such Goryeo celadon was produced mainly in Jeolla Province, which occupies thesouth-western part of the Korean Peninsula, and Gangjin and Buan were the major producingcentres. Goryeo celadon was produced in Gangjin throughout the Goryeo Dynasty (ad 918–1392) and in Buan during the heyday of celadon. In particular, as the sites of the greatestgovernment kilns for Goryeo celadon throughout Korea, Gangjin and Buan in Jeolla Province arelocations that have heightened the technical and artistic value of celadon (Koh-Choo 1995). In

*Received 18 July 2012; accepted 14 January 2013†Corresponding author: email [email protected]

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Archaeometry 56, 3 (2014) 392–405 doi: 10.1111/arcm.12032

© 2013 University of Oxford

mailto:[email protected]

recent years, technical development and production have been implemented for reproduction,with a focus on the colours and shapes of Goryeo celadon, and research has been conducted withdiverse methods to elucidate the technology of Goryeo celadon.

The celadon green colour of Goryeo celadon occurs because unglazed clay and the glaze layerform glassy and crystalline states during the reduction firing process at a high temperature due tochemical reactions (McDevit 1944). The glaze consists of porcelain stone and calcareous woodash, which plays the role of a flux, a glassy coat. In this process, a small quantity of Fe ions playsthe role of a colour developer, thus affecting the chromaticity and gloss of celadon (Zhengyaoet al. 1994; Bin and Zhengyao 2002; Zhang et al. 2004, 2005; Yang et al. 2005). With technologysuch as XPS (X-ray photoelectron spectroscopy), however, it is difficult to observe changes in theelectronic state of the small amount of Fe contained in the specimens. Mössbauer spectroscopyis known to be very useful for measuring the ionic state of celadon glaze containing a smallamount of Fe, amounting to 3% or less (Kim et al. 2010; Lee et al. 2010).

In the present study, the chromaticity of Goryeo celadon pieces excavated at the sites of theGoryeo celadon kilns in Gangjin and Buan in Jeolla Province was measured, and the effectsof the redoxable oxides (Fe2O3, TiO2, MnO and P2O5), which are possibly able to change eachother’s valence states, on the chromaticity of the glaze and the ceramic body were analysed.Furthermore, the correlation between the Fe electronic state of the Goryeo celadon pieces andchromaticity was analysed using Mössbauer spectroscopy and, on the basis of the results of thisanalysis, compared with the results of an experiment on synthetic glaze. In the present work, wehave attempted to elucidate how the physico-chemical properties of celadon are related to thecharacteristic green colour of ancient celadon from the sites of kilns in Gangjin and Buan byspectroscopic methods.

MATERIALS AND METHODS

For the synthetic glaze, in order to realize the colour gamut of the celadon glaze, Fe2O3, TiO2,MnO and P2O5, which are redoxable oxides, were added to the basic glaze to prepare six kindsof glaze recipes. Tables 1 and 2 show the basic glaze recipe and the redoxable oxide recipes. Tominimize the effect of the body on chromaticity, a white porcelain body was used. Dispersants(1 wt% Cerasperse 5468CF by San Nopco, Japan) were added to the basic glaze and mixed in apot mill for 24 h. White porcelain pieces (50 mm ¥ 50 mm), bisque fired at 900°C, were glazedwith six kinds of glaze and reduction fired at 1260°C. When the internal temperature of the

Table 1 The chemical composition of basic glaze

Component Wt%

SiO2 67.42Al2O3 14.28Na2O 0.23K2O 2.5MgO 0.41CaO 14.97Fe2O3 0.11TiO2 0.03P2O5 0.05

The colourative mechanism of Goryeo celadon from GangJin and Buan 393

© 2013 University of Oxford, Archaeometry 56, 3 (2014) 392–405

electric furnace reached 900°C, air/propane-mixed gas was introduced to create a reductionatmosphere. The amount of gas introduced is shown in Table 3.

The Goryeo celadon pieces, which are ancient artefacts (Fig. 1 (a)), were collected from thekiln sites in Gangjin and Buan in Jeolla Province (Fig. 1 (b)), the greatest producing centres ofGoryeo celadon. The specimens of the glaze layer only were isolated from the pieces by abradingthe body part using a mechanical polisher. Body specimens were obtained from the pieces bypolishing the glaze layer. The chromaticity and the Mössbauer spectrum of each layer of the glazeand the body were measured. For the measurement of chromaticity, the L*, a* and b* valueswere obtained using a Minolta CM-700D spectrophotometer, the beam size being adjusted to Ø3–8 mm, and standard tiles were used as the background. Using the obtained chromaticity data,a design of experiment (DOE) analysis was conducted using MINITAB software (Minitab 2007).The Mössbauer spectrum was measured at room temperature using an electrodynamic constantacceleration–type Mössbauer spectrometer and, for the source, a 57Co single source diffusedon the Rh matrix of a Rietverc isotope product (59 mCi) was used. As for the quantity of thespecimen, the density of 57Fe was set at 0.214 mg cm–2, and for homogeneous thickness ofthe specimens, Be plates with a diameter of 1 in and a thickness of 0.005 in were used to coverboth sides.

RESULTS AND DISCUSSION

Analysis of the chromaticity of celadon pieces

The chromaticity values of the body and the glaze layer of the Goryeo celadon pieces excavatedin Gangjin and Buan are shown in Table 4, and Figures 2 (a) and 2 (b) show the colourdistribution of the body (blue) and pieces (black), and of the glaze (black), respectively. The a*value of the body fell between 0.2 and 0.7 and the b* value was between 0.0 and 5.0, showing no

Table 2 The composition of redoxable oxide added to basic glaze

Sample no. Fe2O3 TiO2 MnO P2O5

2 1.40 1.00 0.80 0.3013 2.20 0.10 0.20 0.3018 2.20 0.10 0.20 1.6025 2.20 1.00 0.80 0.3029 2.20 1.00 0.80 0.3034 1.40 0.10 0.20 0.30

Table 3 The conditions of reduction firing

Gas Flow rate

Air 5.0 l min-1

LPG 0.7 l min-1

O2 18.42%

394 A. Y. Jeon et al.


(a)

(b)

(c)

Figure 1 (a) Ancient celadon pieces from the Gangjin and Buan areas. (b) A perspective view of the kiln sites in thevicinity of Gangjin Samheung-Ri. (c) A kiln in the vicinity of Samheung-Ri.



Tabl

e4

The

chro

mat

icit

yan

alys

isof

anci

ent

cela

don

No.

Sam

ple

nam

eA

rea

Age

Bod

yG

laze

L*

a*b*

L*

a*b*

#1/2

YuC

heon

-Ri

(Gye

oRe)

Bua

n12

th–1

3th

cent

urie

sad

62.4

80.

384.

9752

.22

-8.0

47.

41#3

/4Y

ongW

oon-

Ri

(Gye

oRe)

Gan

gJin

10th

cent

ury

ad63

.13

0.22

3.35

70.8

9-4

.27

7.58

#5/6

YuC

heon

-Ri

(5)

Bua

n12

th–1

3th

cent

urie

sad

66.3

00.

491.

8259

.46

-2.8

96.

82#7

/8Y

ongW

oon-

Ri

Gan

gJin

10th

cent

ury

ad62

.62

0.71

4.71

79.9

5-2

.36

4.53

#9/1

0Ss

mhe

ung-

Ri

(E)

Gan

gJin

10th

–11t

hce

ntur

ies

ad58

.99

0.29

4.31

79.6

3-2

.93

3.02

#11/

12Sa

dang

-Ri

(9)

Gan

gJin

12th

cent

ury

ad68

.21

0.21

2.11

65.3

4-3

.70

8.28

#13/

14Sa

mhe

ung-

Ri

(A)

Gan

gJin

10th

–11t

hce

ntur

ies

ad59

.75

0.20

1.63

45.3

4-0

.20

8.41

#15/

16Sa

dang

-Ri

Gan

gJin

12th

cent

ury

ad66

.67

0.22

0.88

63.8

9-7

.38

4.49

#17/

18G

yeE

ul-R

iG

angJ

in67

.74

0.46

1.65

71.9

8-8

.64

6.96



significant changes. On the contrary, the glaze was distributed more broadly than was the body,for the L*, a* and b* values alike.

Figure 3 shows the L*, a* and b* values according to the redoxable oxides of the celadon. Thecomposition of the body was 1.0 wt% or above for Fe2O3 and TiO2, and 0.1 wt% or below forMnO and P2O5, respectively. The composition of the glaze was located at 0.1–3.0 wt% for Fe2O3,TiO2, MnO and P2O5 alike. As a result, while the change in the range of the L* value of the bodywas approximately 1.0, from N5.8 to N6.8, the L* value of the glaze ranged from N4.5 to N7.9,thus exhibiting a change broader than that for the body. In the case of the a* value, while the body

Figure 2 The chromaticity analysis of ancient celadon: (a) an ancient piece of celadon before separation (black) andseparated body (blue); (b) separated glaze.



(a)

(b)

(c)

Figure 3 (a) The evolution of the (a) L* value, (b) a* value and (c) b* value according to the redoxable oxide. The solidand open marks represent glaze and body, respectively.



exhibited values between 0.0 and 1.0, the glaze exhibited values ranging between 0.0 and –10.0.As for the b* value, the body exhibited a range of 0.0–5.0, and the glaze ranged between 0.0 and9.0; thus the range was broader for the glaze than for the body in the cases of the L*, a* and b*values alike.

Table 5 and Figures 4–6 show the results of the DOE analysis of the redoxable oxides ofsynthetic glaze and changes in the L*, a* and b* values according to the Fe2O3 and TiO2 contentin the pieces. Through a DOE analysis of synthetic glaze, the L* value was shown to be affectedby Fe2O3 and TiO2, the a* value by TiO2, and the b* value by Fe2O3, TiO2 and P2O5, which wasindicated by the DOE results (larger values of ‘Effect’, ‘Coefficient’ and T, and small P-values(< 0.05)) in Table 5 (Kim et al. 2011). When changes in the chromaticity of the redoxable oxidesof the pieces were examined (Figs 4 (a) and 4 (b)), the L* value of the glaze was shown to beaffected more by TiO2 than by Fe2O3, and the body was affected more by Fe2O3 than by TiO2. Asshown in Figure 4 (c), unlike the synthetic glaze, the L* value of the glaze in the pieces wasfound to be significantly changed by the amounts of MnO and P2O5. The L* values of the bodyalmost remain unchanged by the amounts of MnO and P2O5 (Fig. 4 (d)). As for the a* value,whereas it was affected by Fe2O3 and TiO2 content in the glaze, there was hardly any change inthe body (Figs 5 (a) and 5 (b)). The a* values of the glaze in the pieces was found to be almostunchanged by the MnO and P2O5 contents, which is consistent with the result of the syntheticsamples (Fig. 5 (c)). As for the b* value, changes due to the content of Fe2O3, TiO2, MnO andP2O5 in the glaze amounted to 5.0–10.0, thus showing a relative decrease in comparison with theL* and a* values, which is unlike the large dependence of the b* value on the Fe2O3 content inthe synthetic glaze (Fig. 6 (a)). For the body, the effect of the redoxable oxides was small, as withthe a* value (Fig. 6 (b)).

Mössbauer analysis

The Mössbauer spectrum of each specimen was analysed with two Fe ion sites, and the results ofthe analysis of each part of the body and the glaze are presented in Table 6. The two sites were

Table 5 The DOE results for the L*, a* and b* values

Terms Effect Coefficient T P-value

L* valuesFe2O3 -5.929 2.9647 7.33 0TiO2 -10.111 5.0553 12.49 0MnO -0.096 0.0478 0.12 0.908P2O5 -0.852 0.4259 1.05 0.309

a* valuesFe2O3 0.998 -0.4998 -1.59 0.132TiO2 7.881 -3.9406 -12.58 0MnO 0.907 -0.4537 -1.45 0.168P2O5 0.124 -0.0619 -0.2 0.846

b* valuesFe2O3 2.1025 -1.0513 -4.43 0TiO2 21.6238 -10.8119 -45.52 0MnO 0.09 -0.045 -0.19 0.852P2O5 1.845 -0.9225 -3.88 0.001



analysed as two resonance absorption lines (line + doublet) exhibiting paramagnetic behaviour,and magnetic behaviour was not observed in any of the specimens measured. The variable dindicates an isomer shift, which in turn represents the Fe ionic valence, ‘Area’ indicates therelative area ratio of Fe2+ and Fe3+ ions, and DEQ indicates the size of the electric quadrupolesplitting.

In Table 6, while the Fe2+/Fe3+ values of the body exhibit a distribution between 2.5 and 9.7,those of the glaze exhibit a distribution between 0.35 and 6.7, and thus the Fe2+/Fe3+ values areapparently greater in the body than in the glaze.

The amount of change in Fe2+/Fe3+ according to the redoxable oxides of the celadon ispresented in Figure 7. As the quantities of TiO2 and Fe2O3 are increased, Fe2+/Fe3+ decreases; andas the quantities of MnO and P2O5 increase, Fe2+/Fe3+ exhibits a slight increase. In particular, thedecrease in Fe2+/Fe3+ due to an increase in the TiO2 content appears to be due to the following: in

Figure 4 (a) The evolution of the L* value for the glaze according to the Fe2O3 and TiO2 contents. The solid, open andcross marks represent glaze, body from ancient celadon and synthetic glaze, respectively. (b) The evolution of the L* valuefor the body according to the Fe2O3 and TiO2 contents. (c) The evolution of the L* value for the glaze according to theMnO and P2O5 contents. (d) The evolution of the L* value for the body according to the MnO and P2O5 contents.



a silicate glassy state, as Ti4+ increases, Fe3+ becomes more stable with respect to Fe2+ (Albertoet al. 1992), and this correlates well with the results for existing synthetic glaze (Kim et al. 2011).Therefore, the Fe2+/Fe3+ value is mainly governed by redox equilibria between Fe and Ti in theglaze layer.

The L*, a* and b* values were analysed according to the amount of Fe2+/Fe3+ obtained byMössbauer spectroscopy (Fig. 8). In the case of the glaze, as the quantity of Fe2+/Fe3+ increased,the a* and b* values in the glaze decreased, indicating a change of colour from red–yellow toblue–green. Unlike a* and b*, the L* values increased slightly (Fig. 8). Such results are highlyconsistent with the changes in the L*, a* and b* values according to Fe2+/Fe3+ in synthetic glaze(Kim et al. 2011). Such an increased L* value (brightness) and decreased a* and b* values

Figure 5 (a) The evolution of the a* value for the glaze according to the Fe2O3 and TiO2 contents. The solid, open andcross marks represent glaze, body from ancient celadon and synthetic glaze, respectively. (b) The evolution of the a* valuefor the body according to the Fe2O3 and TiO2 contents. (c) The evolution of the a* value for the glaze according to theMnO and P2O5 contents. (d) The evolution of the a* value for the body according to the MnO and P2O5 contents.



(blue–green shift) for the glaze are thought to be a source of the characteristic ‘celadon greencolour’.

In contrast to the glaze, as for the body, the breadth of the change in the L* and a* values uponvariation of Fe2+/Fe3+ was negligible (Fig. 8). The b* values for the body increased with Fe2+/Fe3+,although the increase was smaller than that for the glaze. As a result, the colour of celadon isgoverned by the oxidation state of Fe (Fe2+/Fe3+) in the glaze layer, which is affected by thecomposition of the glaze, and especially the TiO2 and Fe2O3 contents, as shown in Figure 7.

CONCLUSION

The chromaticity of the glaze and the body of celadon pieces excavated in Gangjin and Buan inJeolla Province was measured and compared to that of synthetic glaze. In addition, using

Figure 6 (a) The evolution of the b* value for the glaze according to the Fe2O3 and TiO2 contents. The solid, open andcross marks represent glaze, body from ancient celadon and synthetic glaze, respectively. (b) The evolution of the b* valuefor the body according to the Fe2O3 and TiO2 contents. (c) The evolution of the b* value for the glaze according to theMnO and P2O5 contents. (d) The evolution of the b* value for the body according to the MnO and P2O5 contents.



Tabl

e6

The

Mös

sbau

eran

alys

isre

sult

sfo

rth

eG

orye

oce

lado

n

No.

Sam

ple

nam

eA

rea

G/B

Fe3+

Fe2+

Fe2+

/Fe3+

1li

ne(r

edli

ne)

Dou

blet

1(g

reen

line

)

d(m

ms-1

)A

rea

(%)

DEQ

(mm

s-1)

d(m

ms-1

)A

rea

(%)

#1Y

uChe

on-R

i(G

yeoR

e)B

uan

Gla

ze0.

1336

33.9

71.

8949

0.89

5966

.03

1.94

4#2

YuC

heon

-Ri(

Gye

oRe)

Bua

nB

ody

-0.1

228

14.0

31.

8905

0.97

6085

.97

6.12

8#3

Yon

gWoo

n-R

i(G

yeoR

e)G

angJ

inG

laze

0.08

4327

.87

1.85

860.

8812

72.1

32.

588

#4Y

ongW

oon-

Ri(

Gye

oRe)

Gan

gJin

Bod

y-0

.217

712

.55

1.86

891.

0231

87.4

56.

968

#5Y

uChe

on-R

i(5

)B

uan

Gla

ze-0

.031

536

.72

1.74

741.

1020

63.2

81.

7233

#6Y

uChe

on-R

i(5

)B

uan

Bod

y-0

.116

127

.20

1.85

621.

0620

72.8

02.

6765

#7Y

ongW

oon-

Ri

Gan

gJin

Gla

ze0.

1603

74.2

41.

9303

0.95

4025

.76

0.34

70#8

Yon

gWoo

n-R

iG

angJ

inB

ody

-0.2

652

14.1

82.

2936

1.14

9085

.82

6.05

2#9

Sam

heun

g-R

i(E

)G

angJ

inG

laze

0.05

3519

.59

2.17

631.

0848

80.4

14.

105

#10

Sam

heun

g-R

i(E

)G

angJ

inB

ody

-0.2

266

12.9

32.

2937

1.18

3487

.07

6.73

4#1

1Sa

dang

-Ri(

9)G

angJ

inG

laze

0.00

7371

.14

1.55

001.

0292

28.8

60.

4507

#12

Sada

ng-R

i(9)

Gan

gJin

Bod

y-0

.190

69.

331.

8749

0.98

1490

.67

9.71

8#1

3Sa

mhe

ung-

Ri(

A)

Gan

gJin

Gla

ze0.

2033

54.5

12.

0050

0.84

4645

.49

0.83

45#1

4Sa

mhe

ung-

Ri(

A)

Gan

gJin

Bod

y-0

.112

528

.94

1.57

191.

0390

71.0

62.

4554

#15

Sada

ng-R

iG

angJ

inG

laze

-0.0

085

12.8

81.

9185

0.94

3387

.12

6.76

4#1

6Sa

dang

-Ri

Gan

gJin

Bod

y-0

.119

314

.84

2.03

711.

0192

85.1

65.

739

#17

Gye

Eul

-Ri

Gan

gJin

Gla

ze0.

1469

24.4

32.

0156

0.87

3575

.57

3.09

3#1

8G

yeE

ul-R

iG

angJ

inB

ody

-0.0

448

26.2

81.

8280

1.04

8373

.72

2.80

5



Mössbauer spectroscopy, the relationship between the electronic state of Fe and the chromaticityof the glaze and the body of the pieces was analysed. When the chromaticity of the body and theglaze was analysed, the range of the changes in the L*, a* and b* values of the glaze was foundto be broader than in the case of the body; on the other hand, the effect of the body is monotonous,as shown by the small variation of the a* values. According to the results of the chromaticityanalysis, the Fe2O3 content affected the L* and a* values, and the TiO2 content affected the L* anda* values. The MnO and P2O5 contents were found to affect the L* value in the glaze. Accordingto the results of a Mössbauer analysis, the ratio of Fe2+ to Fe3+ was greater for the body than forthe glaze. As the Fe2O3 and TiO2 contents increased, the quantity of Fe2+/Fe3+ decreased; on theother hand, as the MnO and P2O5 contents increased, Fe2+/Fe3+ exhibited little change. As the

Figure 7 The evolution of the ionic state of Fe according to the redoxable oxide.

Figure 8 The evolution of (a) L* and (b) a* and b* according to the ionic state of Fe.



quantity of Fe2+/Fe3+ increased, the a* and b* values in the glaze decreased, indicating a changeof colour from red–yellow to blue–green, and the L* values (brightness) in the glaze increasedslightly.

ACKNOWLEDGEMENT

This study has been conducted as a part of the Establishment of Industrial Technology Founda-tion Project, implemented with support from the Ministry of Knowledge Economy.

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mössbauer spectroscopic and chromaticity analysis on the colourative mechanism of ancient goryeo...

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