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HAL Id: jpa-00249478

https://hal.archives-ouvertes.fr/jpa-00249478

Submitted on 1 Jan 1996

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Photoacoustic Studies of Nanocrystalline Ag and Al2O3

Yuying Huang, Dingchang Xian

To cite this version:

Yuying Huang, Dingchang Xian. Photoacoustic Studies of Nanocrystalline Ag and Al2O3. Journal de Physique III, EDP Sciences, 1996, 6 (5), pp.597-601. �10.1051/jp3:1996142�. �jpa-00249478�

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Photoacoustic Studies of Nanocrystalline Ag and A1203

Yuying Huang and Dingchang Xian (*)

BEPC Synchrotron Radiation Laboratory, Institute of High Energy Physics, Chinese Academy of Sciences, P-O- Box 918, Beijing 100039, P-R- China

(Received 18 July 1994, revised 6 February 1996, accepted 14 February 1996)

PACS.44.30.+v Heat transfer in inhomogeneous media and through interfaces PACS.78.70.Dm X-ray absorption and absorption edges

PACS.81.40.-z Treatment of materials and its effects on microstructures and properties

Abstract. The photoacoustic frequency spectrums of nanocrystalline Ag and A1203 versus the grain size and the annealing temperature respectively were investigated by using synchrotron

radiation X-ray photoacoustic experiments.

1. Introduction

Nanocrystalline materials have also been called ultra-fine grained materials, nanophase mate- rials or nanometer-sized crystalline materials ill. In the case of nanocrystalline materials, the

generation of solids with new atomic structures and properties was attempted by using the atomic arrangements in the cores of defects such as grain boundaries, interphase boundaries or dislocations. Since the atomic structure of nanocrystalline materials differs from the structure of glasses and crystals, the structure-dependent properties of the chemically identical sub-

stances in the glassy or crystalline state, therefore, photoacoustic effect from nanocrystalline

materials may exhibit attractive different features. As we know, the photoacoustic effect has become a subject of intensive research because of its fundamental significance and potential for applications. However, until recently, the photoacoustic technique has been confined in the infrared, visible and ultraviolet regions of the spectrum since the intensity of conventional

light source in the higher energy region is too weak to induce detectable photoacoustic signal.

With the advent of high brilliance synchrotron radiation, it is possible to extend photoacous-

tic technique to the X-ray region of the spectrum. So far photoacoustic effect induced by X-ray absorption from nanocrystalline is still a relative new subject, little attention is paid

to the mechanisms of heat production and transfer in nanocrystalline. This is the purpose of our experiments. In this paper the photoacoustic frequency spectrums of nanocrystalline Ag and A12D3 as a function of the grain size and the annealing temperature respectively was

investigated by using synchrotron radiation X-ray photoacoustic experiments.

(*) Author for correspondence

© Les kditions de Physique 1996

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598 JOURNAL DE PHYSIQUE III N°5

The Sketch of Photoacoustlc Cell

lXMey

Wndow

Mlc

Sample

Wad-

Fig. 1. The sketch of the Photoacoustic cell.

2. Experiments

The experimental arrangement is the same as that shown in the literature [2, 3]. The sketch of the photoacoustic cell for multichromatic synchrotron radiation X-ray experiments is sho~i>n in

Figure I, which was designed for X-ray absorption studies of solid samples, and is similar to the

one described in reference [4]. The brass cell has a volume of18 mm dam. x5 mm, the Beryllium

foil (18 mm dam. x 0.2 mm thickness) was used for the cell windo1N-. The microphone ~i<as a very cheap and commercially available electret condenser type (0.7 mm dam., sensitivity 32 mV/Pa). The chamber was connected to the microphone by a small channel (1 mm dam.

x 7 mm thickness). Samples to be studied were adhered to the inner side of exit Beryllium

1Nindow.

The experimental set-up for X-ray photoacoustic effect is shown in Figure 2. X-ray were chopped by a rotating blade made of Al plate (3 mm thickness), and X-ray photon flux ~vas

monitored by an ion chamber (thickness of Ar gas 2 cm). The photoacoustic signal was fed to an EG&G PARC model 124 lock-in amplifier. The experiments were performed on the wiggler photon beam line 4~V1A (a multichromatic X-ray source, 0.4 3 1) at our laboratory.

The bulk nanocrystalline Ag materials ~i<ere prepared by the inert gas condensation and in sitit compacting technique. The two samples of nanocrystalline Ag have the same diameter 6 mm and thickness 140 ~m with different crystal size 17 nm and 33 nm respectively, which

were studied by TEM (Transmission Electron Nlicroscopy). The nanocrystalline A12D3 clusters

were generated by the chemical reaction method and the bulk ceramics A12D3 were formed

by compacting. The three samples of nanocrystalline A12D3 have the same diameter 12 mm, thickness I-S mm, compacting pressure 150 MPa, and annealing time 4 hours with different

annealing temperature 100 °C, 700 °C and 1280 °C, respectively<.

3. Results and Discuss

The experimental results 1Nere shown in Figures 3 and 4. PAS is the amplitude of photoacoustic signal, f is the chopping frequency. The amplitude of photoacoustic signal of nanocrystalline Ag material with grain size 33 nm is more great than that with 17 nm. The amplitude of

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neExpewnentalsewp

Sin (on Chombei Pholoacouatlc Cell

SR Many

e- Chopper

BEPC Storage Ring

Storage Dacllloscope Loc%In &nplHler

Fig. 2. The experimental set-up for X-ray photoacoustic effect.

PAS versus f

~

m ~

1% , x 17 m ig

_li~ .

33 m fig

W 1.2 .

,o

~

~ x .

g ~ .

~ o~

~ < .

~~ ~'~ X ~

~

~ rn

n_ ~ .

~

15 °.~ ~

~

g~ x .

1 0.4 x

~ .

8 ~

$ 0.2 ~~

fl x~

~ o

I 1.2 lA I-S 1.8 2

Lg(o

Fig. 3. The amplitude of photoacoustic signal (PAS) of nanocrystalline Ag as a function of the

chopping frequency f.

photoacoustic signal of nanocrystalline A12D3 increases as the annealing temperature raises.

It is the basic idea of nanocrystalline materials to generate a new class of disordered solid by introducing a high density of grain boundaries. Nanocrystalline metals exhibit crystal growth

at elevated temperatures. Similar grain growth effects have been noticed in nanocrystalline

ceramics. The density of grain boundaries decreases with grain growth. The photoacoustic

response to X-ray absorption results from the thermalization of the excited Auger electrons and

photoelectrons. The excited electrons have a small mean free path 10-1001 (smaller than the

grain size) and a de Broglie wave length 1-10 1 (much smaller than the grain size). Whereas

we may estimate that the heat production from nanocrystalline may not change much with the

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600 JOURNAL DE PHYSIQUE III N°5

PAS versus f

I-S

$

~ .

i180io iiio3

l% 1.4

x 700 io iiio3

,it

» . a loo io iiio3

W 1.2

~ ~

_g

~

. .

Id

, x x

El 0.8 ''$

I jf ' .x ).

~j o-S ~..

~ .

i 0A

$fi 0.2

#w

0

1.2 lA I.S 1.8 2

Lg(o

Fig. 4. The amplitude of photoacoustic signal (PAS) of nanocrystalline A1203 as a function of the

chopping frequency f.

grain growth. However the thermal diffusion processes may be greatly affected because of a high density of grain boundaries. The thermal resistance increases as the grain size decreases. So in

our experiments the amplitude of photoacoustic signal of nanocrystalline materials decreases

as the grain size decreases. Meanwhile the density of nanocrystalline decreases as the grain

size decreases, therefore the intensity of absorption to X-ray for the samples also decreases.

This may be a factor that reduces the amplitude of photoacoustic signal. These results have shown that thermal wave was intensely scattered by the grain boundaries.

In summary, the photoacoustic frequency spectrums of nanocrystalline Ag and A12D3 uersits

the grain size and the annealing temperature respectively were studied by using synchrotron

radiation X-ray photoacoustic experiments. The production of heat flow resulting from X-ray absorption in the sample is quite different from that resulting from laser absorption. The energy of the X-ray photons is much higher in comparison with the photons from conventional

light sources (laser, xenon lamp, etc.), therefore, for X-ray absorption, heat is mainly generated through excitation and de-excitation of inner shell or core electrons instead of outer shell or

band-gap low-energy electrons. The heat transfer in nanocrystalline Ag and A12D3 is related

to the grain size. The thermal wave was intensely scattered by the grain boundaries. The

photoacoustic effect of nanocrystalline induced by X-ray absorption is still a new field. The heat production mechanisms and diffusion processes are needed to be further investigated for

nanocrystalline with a high density of grain boundaries.

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Acknowledgments

The authors would like to thank Dr. Dong Yuhui and Dr. Zhao Yanming for their meaningful discussions, and Prof. Wu Xijun and Prof. Zhang Lide at Institute of Solid, Chinese Academy

of Sciences for their kind help in providing the experimental nanocrystalline materials. This work is supported by the National Natural Science Foundation of China.

References

ill Gleiter H., Prog. Mat. Sci. 4 (1989) 223.

[2] Yuying Huang et al. In Instrumentation for the First Synchrotron Radiation X-ray Photoa- coustic Experiments in China, Conference Digest and Technical Abstracts of 7th Interna- tional Topical Meeting on Photoacoustic and Photothermal Phenomena (Doorwerth, The

Netherlands, 26-30 August 1991) pp. 373.

[3] Guangming Xiao et al. Photoacoustic Chopping Frequency Response to X-ray Absorption,

Chinese Phys. Lett. 3 (1991) 145.

[4] Masujima T. et al., Rev. Sci. Instritm. 60 (1989) 2318.

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