Fracture Characteristics of Frit Bonding through In-Situ Nano-Indentation Testing

doi:10.1016/j.jmst.2016.09.009

Abstract

Abstract:

Because frit bonding material is brittle, sudden impacts such as dropping may damage the bonding significantly. Strain-rate-controlled in-situ nano-indentation testing, which can determine localized material properties, was carried out on the frit-bonded specimen, especially on the frit bonding matrix and the filler. The results were compared with the drop-impact fracture behavior to understand the fracture characteristics. Mechanical properties at static condition or low strain rate did not show proper relationship with the fracture tendency of the drop tested result of the frit bonding. From the relationship between fracture toughness and the ratio of modulus/hardness, fracture characteristics at the drop impact situation could be estimated by the values at the high strain rate nano-indentation. The ratio between modulus and hardness on frit matrix showed close relationship with drop impact fracture. Though crack propagation path deflected at filler interface, filler property gave less influence on fracture tendency of drop impact fracture due to its small volume fraction. The properties of frit matrix were crucial to the fracture characteristics of the frit bonding.

Key words: Nanoindentation, Bonding, Fracture behavior

Je Jo Won,Ahn Hee-Jun,Hyoung Kim Jong,Kwon Dongil. Fracture Characteristics of Frit Bonding through In-Situ Nano-Indentation Testing[J]. J. Mater. Sci. Technol., 2016, 32(11): 1204-1210.

Figures/Tables 12

Fig. 1. Indentation load-displacement curve.

Fig. 2. Schematic structure of frit bonding (a), and SEM micrograph of frit bonding (b).

Fig. 3. Drop impact test apparatus.

Fig. 4. In-situ nano indentation test (a) in the frit bonding matrix (b), and in the filler (c).

Fig. 5. Indentation load-displacement curves of frit material: (a) V-T-based frit bonding matrix; (b) V-T-based frit bonding filler; (c) V-P-based frit bonding matrix; (d) V-T-based frit bonding filler; (e) Bi-based frit bonding matrix; (f) Bi-based frit bonding filler.

Fig. 6. Revealed crack like morphology within indented surface: V-T-based frit bonding; V-P-based frit bonding; (c) Bi-based frit bonding; (d) schematic of crack like morphology.

Table 1. In-situ nano indentation results of frit bonding specimen

	VT based bonding specimen ---------------					VP based bonding specimen --------------					Bi based bonding specimen -----------------
	E (GPa)	err	H (GPa)	err	E/H	E (GPa)	err	H (Gpa)	err	E/H	E (GPa)	err	H (GPa)	err	E/H
Filler	74.43	4.19	2.60	0.51	28.6	136.6	3.34	3.57	0.39	38.2	112.5	3.53	3.69	0.25	30.5
Matrix	50.35	2.65	2.56	0.16	19.6	49.4	3.98	2.67	0.19	18.5	68.79	3.39	3.20	0.13	21.5
Drop fracture resistance	High					Middle					Low

Table 2. In-situ nano indentation results with various strain rates

Strain rate (s)	VT based bonding specimen(matrix) --------------					VP based bonding specimen(matrix) -----------------					Bi based bonding specimen(matrix) -----------------
Strain rate (s)	E (GPa)	err	H (GPa)	err	E/H	E (GPa)	err	H (GPa)	err	E/H	E (GPa)	err	H (GPa)	err	E/H
1	50.35	2.65	2.56	0.16	19.66	49.46	3.98	2.67	0.19	18.52	68.78	3.39	3.20	0.12	21.46
10	51.35	3.27	2.62	0.26	19.59	51.12	1.84	2.71	0.04	18.86	65.42	3.12	3.50	0.22	18.66
15	53.22	1.23	2.82	0.02	18.87	53.72	1.63	2.86	0.02	18.78	67.88	1.33	3.94	0.11	17.22
25	69.34	5.766	3.63	0.3	19.10	72.21	1.76	4.12	0.26	17.52	69.22	1.44	4.43	0.13	15.62

Fig. 7. Indentation hardness (a) and elastic modulus (b) with various strain rates.

Fig. 8. E/H ratio with various strain rates.

Fig. 9. Crack propagation of frit bonding matrix after drop impact test.

Fig. 10. Crack propagation in the matrix and along filler-matrix interface: (a) advancing crack deflected by filler particle; (b) crack branching occurred as the advancing crack met the filler particles.

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