KR101783427B1 - Method for controlling of growth of self-assembled Au nanoparticles on GaN - Google Patents
Method for controlling of growth of self-assembled Au nanoparticles on GaN Download PDFInfo
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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
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- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
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Abstract
According to an aspect of the present invention, there is provided a method of manufacturing a GaN substrate, A gold deposition step of depositing gold on the prepared GaN substrate; And a gold nanoparticle deposition step of spontaneously forming gold nanoparticles deposited on the GaN substrate through a heat treatment process at an annealing temperature of 400 to 800 DEG C for 300 +/- 30 seconds; Wherein the shape, size, and density of the spontaneously-formed gold nanoparticles are controlled by controlling the annealing temperature to control the growth of gold nanoparticles spontaneously formed on the GaN.
Description
The present invention relates to a method for controlling the growth of gold nanoparticles spontaneously formed on GaN.
Au nanoclusters and nanoparticles are widely used in a variety of electronic, optoelectronic, and bio-medical fields due to their great potential. The size, density, and composition of gold nanoparticles play an important role in the performance of these devices.
Recently, gold nanoparticles have attracted major research attention due to their potential applications in solar cells, memory, sensors, and bio-medical devices due to localized surface plasmon resonance, increased absorption, enhanced fluorescence and scattering. The performance of the corresponding devices is strongly dependent on the size and density of gold nanoparticles.
For example, gold nanoparticles exhibit localized surface plasmon resonance properties that enhance the absorption of light, thus providing meaningful improvements in the efficiency of the solar cell. Relatively large gold nanoparticles can achieve higher power conversion efficiencies. On the other hand, small-sized gold nanoparticles with increased density have the potential to improve the turn-on voltage and on / off current ratio in nanofiber-based memory devices
In addition, arrays of large gold nanoparticles of spherical shape can be used in the manufacture of lasers for sensing applications. Gold nanoparticles can also be used to improve performance for DNA detection in biomedical devices because they can increase fluorescence intensity.
Gold nanoparticles may also be implemented in quantum-thermal therapy and cancer diagnosis due to enhanced radioactivity properties such as absorption and scattering by strong electromagnetic fields on the particle surface.
On the other hand, the performance and lifetime of a semiconductor device such as a laser diode and a light emitting diode are determined by various factors constituting the device. In particular, the performance and the lifetime of the device are greatly affected by the base substrate on which the devices are stacked. Accordingly, various methods for manufacturing a high-quality semiconductor substrate have been proposed. Recently, interest in III-V compound semiconductor substrates has increased.
Here, a typical III-V compound semiconductor substrate is a gallium nitride substrate, and a gallium nitride substrate is suitably used for a semiconductor device together with a GaAs substrate, an InP substrate, and the like.
In addition, because of its wide bandgap, strong chemical bonding, high electrical breakdown voltage, high electronic mobility and high melting point, GaN is high in high power devices such as UV LEDs, photovoltaics, power amplifiers, transistors and opto-bandgap optoelectronic devices. Attracting attention.
Although we are studying the application of gold nanoparticles on GaN for the development direction of many applications, systematic studies on the control of shape, size and density of gold nanoparticles on GaN (0001) are insufficient.
In order to precisely manufacture nanowires for various applications, a method of controlling the size and density of gold nanoparticles on GaN (0001) is required.
Prior art in this field is disclosed in Korean Patent Registration No. 10-1287611.
The present invention provides a growth control method for shape, size, and density of spontaneously-formed Au nanoparticles by controlling an annealing temperature in a growth process on a GaN substrate.
The object of the present invention is not limited to the above-mentioned objects, and other objects not mentioned can be clearly understood from the following description.
According to an aspect of the present invention, there is provided a method of manufacturing a GaN substrate, A gold deposition step of depositing gold on the prepared GaN substrate; A gold nanoparticle growth step in which gold nanoparticles are spontaneously formed on the sapphire GaN substrate through a heat treatment process at an annealing temperature of 400 to 800 DEG C for 300 +/- 30 seconds after the gold deposition step; And controlling the annealing temperature to control the shape, size, and density of the spontaneously formed gold nanoparticles. The method for controlling growth of spontaneously formed gold nanoparticles on GaN is provided.
The gold nanoparticles are spontaneously formed on the (0001) plane of the GaN substrate.
The GaN substrate preparation step may include: preparing a GaN wafer having a thickness of 10 2 탆 thick on a sapphire substrate having an off-axis of ± 0.1 °; And the GaN wafer is indium-bonded in an Inconel holder and is cleaned in a pulsed laser deposition chamber for 0.5 to 1 hour in a Torr atmosphere at 650-750 ° C and 1 × 10 -4 × (± 10%); And a control unit.
The gold deposition step may be performed in a plasma ion-coater chamber in which the ionization current is in the range of 1 × 10 -1 × (± 10%) torr and in the range of 3 to 5 mA, and 0.05 ± 0.01 nms -1 . ≪ / RTI >
The gold nanoparticle growth step may be performed by performing a heat treatment process at a ramping rate of 2.2 to 2.4 ° C s -1 in a PLD chamber of 1 × 10 -4 × (± 10%) Torr atmosphere .
Further, the method further includes the step of quenching the temperature in the PLD chamber to room temperature after the gold nanoparticle growing step.
Also, the annealing temperature is increased to control the size of the spontaneously formed gold nanoparticles to be increased and the density to decrease.
In addition, gold is deposited to a thickness of 5 ± 0.5 nm in the gold deposition step, and the annealing temperature is controlled to 400 ° C. in the growth step to form hexavalent voids in the spontaneously-formed gold nanoparticles do.
The depth of the hexagonal void is 7 to 9 nm.
In addition, gold is deposited to a thickness of 5 ± 0.5 nm in the gold deposition step, and the annealing temperature is controlled to 500 ° C. in the growth step to deposit hexagonal gold nanoparticles having a depth of 11 to 13 nm Thereby forming voids.
In addition, gold is deposited to a thickness of 5 ± 0.5 nm in the gold deposition step, and the annealing temperature is controlled to 600 ° C. in the growth step to form spontaneous-formed gold nanoclusters.
In addition, gold is deposited to a thickness of 5 ± 0.5 nm in the gold deposition step, and the annealing temperature is controlled to 650 ° C. in the growth step to form small dome spontaneously-formed gold nanoclusters .
The physical properties of the spontaneously formed gold nanoclusters have an average height of 59.2 to 71.2 nm, an average density of 7.4 to 9.0 × 10 8 cm -2 and a side diameter of 155.4 to 180.4 nm.
The average height of the gold nanoparticles is increased by 1.8 to 2.1 times and the side thickness is increased by 1.7 to 2.0 times as compared with the physical properties in which the annealing temperature is controlled to 700 占 폚 and the annealing temperature is controlled to 650 占 폚 And the average density is controlled to decrease in a ratio of 5.15 to 5.30 times.
The average height of the gold nanoparticles was increased by 0.95 to 1.25 times and the side thickness thereof was increased by 1.00 to 1.20 times, And the density is controlled to decrease in a ratio of 1.90 to 2.32 times.
In addition, in the gold deposition step, gold of 5 ± 0.5 nm is deposited, and the annealing temperature is controlled to 800 ° C. in the growth step. The average height of the spontaneously formed gold nanoparticles is 134.5 to 165.5 nm and the average density is 5.4 To 6.6 × 10 7 , and the side diameter is controlled to be 352.5 to 412.5 nm.
According to one embodiment of the present invention, the shape, size, and density of spontaneously-formed gold nanoparticles on GaN can be controlled by controlling the annealing temperature during the growth process on the GaN substrate.
As the annealing temperature increases, the shape, size, and density of spontaneously-formed gold nanoparticles can be controlled by increasing the size of the spontaneously-formed gold nanoparticles while decreasing the density.
Figure 1 shows a method for the production of hexagonal gold voids, nano-clusters and nanoparticles spontaneously formed on GaN (0001).
FIG. 2 shows the growth pattern of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 400 ° C. to 600 ° C. after 5 nm gold deposition.
Figure 3 shows the growth pattern of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 650 ° C to 800 ° C after 5 nm gold deposition.
Figure 4 graphically shows the physical properties of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 650 ° C to 800 ° C after 5 nm gold deposition.
FIG. 5 shows the growth pattern of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 700 ° C. to 800 ° C. after 10 nm gold deposition.
Figure 6 shows the EDS maps, spectra, and line profiles of spontaneously formed gold nanoparticles with 10 nm of gold deposition annealed at 750 < 0 > C for 300 seconds.
FIG. 7 shows the growth pattern of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 650 ° C to 800 ° C after 4 nm gold deposition.
FIG. 8 is a graph showing changes in average height (A H ), side diameter (L D ), and average density (A D ) for each annealing temperature change of spontaneously formed nanoparticles with a deposition thickness of 4, will be.
The terminology used in this application is used only to describe a specific embodiment and is not intended to limit the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise.
In the present application, when a component is referred to as "comprising ", it means that it can include other components as well, without excluding other components unless specifically stated otherwise. Also, throughout the specification, the term "on" means to be located above or below the object portion, and does not necessarily mean that the object is located on the upper side with respect to the gravitational direction.
According to an embodiment of the present invention, there is provided a method of manufacturing nanostructured and spontaneously-formed gold nanoparticles on GaN while varying the annealing temperature (Ta) and the deposition amount (DA).
According to another embodiment of the present invention, at a relatively low annealing temperature of 400 ° C to 800 ° C compared to the prior art, hexagonal shaped gold voids and gold nano- Configuration is provided.
According to one embodiment of the present invention, the fabrication of spontaneously-formed gold nanoparticles and nanostructures on GaN (0001) with varying annealing temperature and deposition amounts presents various growth conditions.
A GaN (0001) substrate according to an embodiment of the present invention is prepared with a GaN wafer having a thickness of 10 + - 2 [mu] m-thick grown on sapphire having off axis ± 0.1 [deg.].
GaN wafer according to one embodiment of the present invention is Inconel holder to indium is coupled, since the removal of contamination on the surface, for degassing at 1 × 10 4 x (± 10 %) 650 ~ 750 ℃ under Torr 0.5 ~ 1 The cleaning process may be performed in a pulsed laser deposition (PLD) chamber for a period of time.
Various quantities of gold are then deposited on the samples in the ion-coater chamber at an ionization current of 3 to 5 mA and a growth rate of 0.05 +/- 0.01 nm / s under 1 x 10 -1 (10%) Torr.
The gold nanoparticle growth step is followed by a heat treatment at a ramping rate of 2.2-2.4 ° C s -1 in a PLD chamber of 1 × 10 -4 × (± 10%) Torr atmosphere after the gold deposition step .
In one embodiment of the present invention, a constant deposition amount and a control characteristic at an annealing time are shown for a series of samples in order to clearly realize annealing temperature effect characteristics for spontaneously formed gold nanoparticles and nanostructures.
Figure 1 shows a method for the production of hexagonal gold voids, nano-clusters and nanoparticles spontaneously formed on GaN (0001).
Referring to FIG. 1, a method of fabricating hexagonal gold voids and spontaneously-formed gold nanostructures is performed by changing the annealing temperature to 400 to 800 ° C.
The variation of the annealing according to one embodiment of the present invention is systematically performed between 400 and 800 ° C with a fixed deposition amount and an annealing time.
The annealing process is performed in a PLD chamber having the same ramping rate of 2.2 DEG to 2.4 DEG C / s for each series under 1 x 10 4 x (10%) Torr.
After each target temperature is reached, a growth process for 300 +/- 30 seconds is performed.
Here, ± 30 seconds means the error range of the process.
After each growth settling, the temperature is immediately quenched to room temperature to minimize Ostwald ripening.
FIG. 1 (a) shows an atomic force microscopy (AFM) top view of a bare surface. FIG. 1 (b) It is.
FIG. 1 (c) shows a surface morphology in which a growth process is performed at an annealing temperature of 400.degree. C. for 300. + -. 30 seconds.
FIG. 1 (d) shows a surface morphology in which a growth process was performed at an annealing temperature of 600 ° C. for 300 ± 30 seconds.
FIG. 1 (e) shows a surface morphology in which a growth process is performed at an annealing temperature of 750 ° C. for 300 ± 30 seconds.
According to an embodiment of the present invention, the AFM top-views (a) and (b) in FIG. 1 represent a size of 1 × 1 μm 2 and the AFM top- 2 size.
1 (a-1) to (e-1) show cross-sectional profiles of transverse white lines (a) to (e).
FIG. 1 (c-2) is an enlarged view of the green square portion in FIG. 1 (c), which shows the shape of a hexagonally formed void.
Fig. 1 (c-3) shows the crystal structure of atoms of GaN (0001).
FIG. 1 (d-2) shows a gold nanocluster spontaneously formed by enlarging a green square portion in FIG. 1 (d).
FIG. 1 (e-2) shows a gold nanocluster spontaneously formed by enlarging a green square portion in FIG. 1 (e).
The surface morphology of the deposited film becomes slightly rugged as compared to the bare surface as shown in the cross-sectional line-profile of Figs. 1 (a-1) and (b-1).
As shown in FIG. 1 (c), hexagonal gold voids are formed after annealing at 400 ° C. for 300 ± 30 seconds.
Also, as shown in Fig. 1 (d), gold nanoclusters are formed after annealing at 600 DEG C for 300 +/- 30 seconds.
Also, as shown in Fig. 1 (e), spontaneously formed gold nanoparticles having distinct sizes are formed after annealing at 750 DEG C for 300 +/- 30 seconds.
Figure 2 shows the growth pattern of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 400 ° C to 600 ° C after 5 ± 0.5 nm gold deposition.
2 (a) to 2 (c) show the results of deposition of gold of 5 ± 0.5 nm, respectively, and then deposition of gold at 500 ° C. (FIG. 2 (a) 2 shows the spontaneous-formed growth pattern of gold nanoparticles deposited on GaN (0001) for 300 < RTI ID = 0.0 > 30s < / RTI > at annealing temperature of 600 ° C (FIG.
Here, ± 0.5 nm means an error range generated in the process execution.
2 (a-1) to (c-1) show cross-sectional profiles for the cross-section of the inner square line.
2 (a-2) to (c-2) show FFT power spectra of particles generated under each condition.
Referring to FIG. 2, as the annealing temperature (Ta) is increased, the size of the void increases and the density of the void decreases accordingly.
Further, referring to Fig. 2 (a), small voids are initially formed, they are tightly coupled and coupled, and when the size of the voids becomes larger, the voids appear separately as shown in Fig. 2 (b).
Further, by further increasing the annealing temperature (Ta), an irregular shape of gold nano-clusters is formed as shown in Fig. 2 (c). The formation of the nano-clusters in Fig. 2 (c) can be attributed to the increase in the size of the voids by bonding adjacent ones, resulting in isolated regions of gold being analyzed.
According to one embodiment of the present invention, hexagonal gold voids and spontaneously formed gold nano-particles formed spontaneously on GaN (0001) while varying the annealing temperature from 400 ° C to 600 ° C for 300 ± 30 seconds after a 5 nm thick gold deposition step, Cluster, and so on.
The growth of spontaneously formed gold voids, nanoclusters and gold nanoparticles on GaN (0001) is analyzed to be related to thermodynamics between annealing temperature, surface diffusion coefficient and diffusion length.
The surface diffusion coefficient (Ds) follows the following scaling relation.
[Formula 1]
D s ? Exp (- En / KTa)
Where En is the diffusion barrier, K is the Boltzmann constant and Ta is the annealing temperature.
Thus, the surface diffusion coefficient is directly related to the annealing temperature.
Further, the diffusion length (L D ) can be obtained by the following equation (2).
[Formula 2]
L D = √ (D s t),
Where t represents the diffusion time.
Referring to
In one embodiment with an annealing temperature of 400 캜, gold adsorbing atoms (adatoms) can be diffused to coalesce with other gold adsorbing atoms (adatoms) by thermal energy of 400 캜.
However, due to insufficient or low thermal energy, shortened diffusion lengths can lead to suppression or impairment of aggregation or diffusion of gold adsorbing atoms (adatoms).
As a result, hexagonal voids can be formed in the gold layer on the GaN as shown in Fig. 2 (a). Referring to the cross-sectional surface line profile of Figure 2 (a-1), the depth of the void is approximately 7 to 9 nm.
As shown in Fig. 1 (c-3), the crystal structure of GaN (0001) is hexagonal with Ga and N connected to each other, and thus the overall structure for voids is also hexagonal.
After annealing at 400 ° C, gold atoms diffuse thermal energy. The adsorption of gold adsorbed atoms on the gold adsorbed atoms (adatoms) is then regrouped to form a top-terminated hexagonal close packed (hcp) -GaN crystal structure. I have.
Thus, the hexagonal voids formed on the gold layer on GaN (0001) can be formed by the influence of the crystal structure of GaN (0001).
Increasing the annealing temperature to 500 占 폚 as in the embodiment of FIG. 2 (b), the diffusion length is increased and the gold adsorbing atoms (adatoms) can be further agglomerated.
And as a result, as shown in FIG. 2 (b), the size of the void is increased and the density is decreased. It can be seen that the depth of the voids is increased from 11 to 13 nm when referring to the cross-sectional surface line profile in Fig. 2 (b-1).
As shown in FIG. 2 (C), due to the increased diffusion length at the annealing temperature of 600 ° C., gold clusters are grown on the basis of diffusion limited aggregation (DLA) characteristics.
The DLS property means that random walk adsorption atoms (Adatoms) due to Brownian motion will aggregate to form gold clusters with enhanced surface diffusion.
As shown by the cross-sectional line profile in (a-1) to (c-1) of FIG. 2, the height of the gold clusters rapidly increased from less than 10 nanometers to more than one hundred nanometers.
The surface morphology can be described by the FFT power spectra shown in (a-2) to (c-2) in FIG.
Referring to FIG. 2 (a-2), at an annealing temperature of 400 ° C., the FFT power spectrum shows a bright hexagonal pattern due to the formation of hexagonal voids and similarly the increased size of hexagonal voids.
Further, referring to (a-2) of FIG. 2, the FFT power spectra at the annealing temperature of 500 ° C becomes smaller and fainter.
It is also possible to refer to (c-2) in FIG. At an annealing temperature of 600 [deg.] C, irregularly shaped gold nano-clusters are formed, and the FFT power spectra become round and faint.
FIG. 3 shows the growth pattern of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 650 ° C. to 800 ° C. after 5 ± 0.5 nm gold deposition.
3 (a) to 3 (d) are graphs showing the results of the deposition of gold of 5 ± 0.5 nm and the deposition of gold at 650 ° C. (FIG. 3 (a)), 700 ° C. (FIG. (0001) at an annealing temperature of 750 캜 (Fig. 3 (c)) and 800 캜 (Fig. 3 (d)) for 300 賊 30 s.
3 (a) to (d) show AFM top-views at an area of 20 × 20 μm 2 and an area of 5 × 5 μm 2 at an annealing temperature of 650 ° C. to 800 ° C., respectively.
3 (a-1) to (d-1) show cross-sectional profiles for cross-sectional views of internal square lines of small area portions at 650 ° C to 800 ° C annealing temperatures, respectively.
3 (a-2) to (d-2) show FFT power spectra of particles generated at an annealing temperature of 650 ° C to 800 ° C, respectively.
4 graphically illustrates the physical properties of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 650 ° C to 800 ° C after 5 ± 0.5 nm gold deposition.
Referring to FIG. 4, it can be seen that as the annealing temperature (Ta) increases after gold deposition, the size of the gold nanoparticles is also increased while the density is decreased.
Referring to Figs. 3 and 4, initially, dome-shaped small size and dense agglomerated gold nanoparticles are observed in Fig. 3 (a).
In Fig. 3 (b), when the annealing temperature is increased to 700 캜, the gold nanoparticles grow, are spaced apart, and the density is further reduced.
In Fig. 3 (c), the size of the gold nanoparticles also increases, the isolated spacing increases and the density decreases.
As shown in Fig. 3 (d), when the temperature is increased to 800 ° C, the gold nanoparticles are much larger in size and less dense.
If the binding energy E A between the gold adsorbing atoms (adatoms) is greater than the gold adsorbing atoms (adatoms) and the binding energy E G between Ga and N atoms (i.e. E A > E G ) Adatoms can bond strongly to each other and can form spontaneously formed 3-D islands like gold nanoparticles on GaN with sufficient diffusion energy provided.
By increasing the annealing temperature, the diffusion length (L D ) can be increased so that the island can absorb more gold adsorbing atoms (adatoms), the size of the nanoparticles can be increased and the density can be reduced.
This is because when nanoparticles increase, smaller nanoparticles, due to lower surface energy, tend to be attracted to form larger nanoparticles until they reach equilibrium.
Plots of mean height (A H ), mean density (A D ), and side diameter (L D ) of spontaneously formed gold nanoparticles are shown in Figures 4 (e) and 3 (f).
Referring to FIG. 4, small dome-shaped self-assembled gold nanoparticles were initially observed at 650 ° C, and A H , A D and L D were 65.2 nm, 8.2 × 108 cm -2 and 165.4 nm, respectively.
The A H , A D , and L D distributions of the gold nanoparticles were found to be 59.2 to 71.2 nm, 7.4 to 9.08 108 cm -2 and 155.4 to 180.4 nm at 650 ° C., respectively, according to one embodiment of the present invention. .
After increasing the Ta to 700 ° C, the A H increased 130.2 nm to 1.99 times that of 650 ° C, the L D increased 1.86 times to 309.1 nm, and the A D dropped 5.25 times to 1.56 × 10 8 / cm 2 .
The AH was increased by 1.8 to 2.1 times, the LD was increased by 1.7 to 2.0 times, and the AD was increased by 5.15 to 5.30 times fell.
When the Ta was further increased to 750 ° C, A H and L D were also increased 1.12 times to 146.2 nm and 1.10 times to 341.4 nm, respectively, compared with 700 ° C, and the A D decreased 2.11 times to 7.2 × 10 7 cm -2 .
The AH and LD values were increased from 0.95 to 1.25 times and 1.00 to 1.20 times, respectively, and the AD was 1.90 to 2.32 times higher than that at 700 ° C by further increasing the temperature range from 700 ° C. to 750 ° C. Respectively.
Furthermore, at an annealing temperature of 800 ° C, the size of gold nanoparticles grew further and the density continued to drop. At an annealing temperature of 800 占 폚, A H is 149.6 nm, L D is 382.4 nm, and A D is 6 × 10 7 / cm 2 .
The A H is 134.5 to 165.5 nm, the L D is 352.5 to 412.5 nm, and the A D is 5.4 to 6.6 × 10 7 /
Overall, in the gold deposition of 5 ± 0.5 nm, the A H and L D increased 2.29 times and 2.31 times and the A D decreased 13.66 times between annealing temperatures of 650 and 800 ° C, respectively.
In the average distribution according to an embodiment of the present invention, AH and LD were increased 2.14 to 2.35 times and 2.16 to 2.46 times and annealing temperature was decreased 12 to 14 times Respectively.
According to an embodiment of the present invention, the shape, size, and density of the spontaneously-formed gold nanoparticles can be controlled by controlling the physical properties of the nanoparticles through the control of the annealing temperature in the range of 400 to 800 ° C.
3 (a-2) to (d-2), the FFT spectrum is much wider in FIG. 3 (a-2) due to the wide distribution of the height of the gold nanoparticles, Lt; RTI ID = 0.0 > 800 C, < / RTI > the FFT spectra exhibit similar size uniformity and all appear similar.
Figure 5 shows the growth pattern of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 700 ° C to 800 ° C after 10 ± 1 nm gold deposition.
5 (a) to 5 (d) show the results of deposition of gold of 10 1 nm and deposition of gold at 700 ° C (FIG. 5A), 750 ° C. (FIG. Shows the growth pattern of spontaneously-formed gold on GaN (0001) for each 300 +/- 30s at an annealing temperature of 800 DEG C (FIG. 5 (c)).
5 (a) to (c) show AFM top-views at an area of 20 × 20 μm 2 and an area of 5 × 5 μm 2 at an annealing temperature of 700 ° C. to 800 ° C., respectively.
5 (a-1) to (c-1) show cross-sectional profiles for the cross-section of the inner square line of a small area portion at an annealing temperature of 700 ° C to 800 ° C, respectively.
5 (a-2) to (c-2) show FFT power spectra of particles generated at an annealing temperature of 700 ° C to 800 ° C, respectively.
Referring to FIG. 5, as in the growth process at the time of 5 ± 0.5 nm deposition, A H and L D of gold nanoparticles were increased with increasing Ta and A D gradually decreased.
Referring to Figure 5 (a), at 700 ° C annealing, the gold nanoparticles exhibit a uniform dome-shaped size.
Referring to FIG. 5 (b), the gold nanoparticles slightly increased in size and decreased in density as compared with (a).
In FIG. 5 (c), the gold nanoparticles are larger and the density is lower than that of (b).
Referring to FIGS. 5 (a-1) to (c-1), the size evolution of spontaneously formed gold nanoparticles with an increased annealing temperature can be seen.
Referring to Figures 5 (a-2) to (c-2), it can be seen that the FFT power spectra are only slightly changed in size and brightness due to small variations in the uniformity and height distribution of the gold nanoparticles .
Figure 6 shows the EDS maps, spectra, and line profiles of spontaneously formed gold nanoparticles with 10 1 nm gold deposition annealed at 750 ° C for 300 ± 30 seconds.
The morphology of spontaneously formed gold nanoparticles is shown in the SEM image of FIG. 6 (a) and the corresponding gold 2-D phase map is shown in FIG. 6, 5 (b).
Also, a 3-D plan view of the Au and Ga component maps is shown in Figures 6 (c) and 5 (d). Referring to FIG. 6, the 2-D phase of gold (Au) is represented by a gold concentration level according to color. The red area has the highest gold concentration, the yellow has a slightly lower concentration, and the green has a lower gold content.
Further, the blue region indicates that gold is not present or is extremely small.
Referring to FIG. 6, the peak represents the gold (Au) count while the remaining region is Ga. In the 3-D plan view of the Ga map, the holes represent gold and the remaining portion represents Ga.
The concentration of gold in a particular region is illustrated by EDS spectra and line-profiles, as shown in Figures 6 (e) - (h).
For example, gold (Au) peaks in the gold nanoparticle region in the EDS spectra and line-profile show higher counts in the absence of nanoparticles.
FIG. 7 shows the growth pattern of spontaneously-formed gold on GaN (0001) when the annealing temperature is changed from 650 ° C. to 800 ° C. after 4 ± 0.5 nm gold deposition.
7 (a) to 7 (d) show the results of deposition of gold of 4 ± 0.5 nm, respectively, after 650 ° C. (FIG. 7 (a)), 700 ° C. (FIG. 7 (0001) at 300 ° C for 30 seconds at an annealing temperature of 750 ° C (Fig. 7 (c)) and 800 ° C (Fig. 3 (d)).
7 (a) to (d) show AFM top-views at 20 × 20 μm 2 area and 5 × 5 μm 2 area at 650 ° C. to 800 ° C. annealing temperature respectively after depositing 4 ± 0.5 nm gold .
7 (a-1) to (d-1) show the cross-sectional profile of the cross-section of the inner square line of the small area portion at 650 ° C to 800 ° C annealing temperature after each deposition of 4 ± 0.5 nm gold will be.
7 (a-2) to (d-2) show the FFT power spectra of particles generated at 650 ° C. to 800 ° C. annealing temperature after deposition of 4 ± 0.5 nm gold, respectively.
The gold nanoparticles have a pattern similar to the deposition pattern of the different thicknesses described above for the Ta change. The A H and L D of gold nanoparticles increase as Ta increases, and A D decreases gradually.
Referring to FIG. 7, in the case of 4 ± 0.5 nm gold deposition, A H , L D and A D of spontaneously formed gold nanoparticles at 650 ° C. were 47.7 nm, 136.1 nm and 2.7 × 10 9 cm -2, respectively. After annealing at 700 ° C, the A H of gold nanoparticles increased by 1.08 times to 51.9 nm, the L D increased by 1.15 times to 156.8 nm, and the A D decreased by 2.43 times to 1.11 × 10 9 cm -2 .
In summary, according to the distribution according to an embodiment of the present invention,
At 750 ° C, the A H and L D were found to be 80.1 and 213.9 nm, and the A D was 7.36 × 10 8 cm -2 . At 800 ° C., the A H decreased by 1.27 times to 62.8 nm and the L D was 252.3 nm 1.17 times and A D was 6.24 × 10 8 cm -2 and decreased by 1.17 times.
Therefore, it can be seen that the height of the gold nanoparticles having the deposition thickness of 5 nm and 10 nm is increased while the height of the gold nanoparticles having the deposition thickness of 4 nm is decreased at the Ta of 800 ° C.
This may be due to the loss of nitrogen from GaN and surface disorder at higher temperatures and is more apparent at lower deposition thicknesses of 4 nm.
FIG. 8 is a graph showing changes in average height (A H ), side diameter (L D ), and average density (A D ) for each annealing temperature change of spontaneously formed nanoparticles with a deposition thickness of 4, will be.
4, 5, and 10 nm deposition thicknesses (DA) showed a similar evolutionary tendency to spontaneously formed gold nanoparticles, with increasing A H and L D as a function of Ta and decreasing A D.
Overall, as gold deposition increases, relatively large sizes of gold nanoparticles are formed.
For example, a 10 nm thick line is always above the 5 nm thick line on the A H and L D plots, and similarly a 5 nm thick line is always above the 4 nm thick line.
Also, density plots are reversed, with larger nanoparticles exhibiting lower densities as mentioned above.
As described above, the diffusion length is determined by Ta, and by increasing the deposition amount at a specific temperature, more adsorbed atoms (adatoms) can be absorbed in the initially formed nanoparticles.
Given greater binding energy (EA > EG) and sufficient thermal energy, the nanoparticles may become larger and, as the side diameter increases, they may pour the absorption boundary and grow further until equilibrium is reached do.
Similar results can also be observed from gold nanoparticles on GaAs and platinum nanoparticles on Si substrates, but the growth conditions are: 550 ° C for 150 seconds of Au / GaAs, and round dome shape at 800 ° C for 240 seconds of Pt / Si Of the nanoparticles are produced, and also vary from substrate to substrate, respectively.
According to one embodiment of the present invention, Ta is controlled with a deposition amount of 4, 5, 10 nm of gold to control the physical properties and shape of spontaneously formed hexagonal gold voids, nano-clusters and nanoparticles on GaN (0001) .
According to one embodiment of the present invention, nucleation of voids and clusters can be implemented at annealing temperatures of 400 and 600 ° C for 300 ± 30 seconds and can be analyzed based on diffusion limited cohesive properties.
According to one embodiment of the present invention, by increasing the Ta to 600 占 폚, the void size of spontaneously formed gold particles is increased and the density is reduced.
According to one embodiment of the present invention, when the annealing temperature is increased to 600 ° C, the spontaneously formed gold clusters are evolved to distinct sizes, and when the Ta is further increased to 650 ° C, spontaneously formed gold nanoparticles grow into Volmer-Weber growth It evolves according to the model.
Claims (17)
A gold deposition step of depositing gold on the prepared GaN substrate;
A gold nanoparticle growth step in which gold nanoparticles are spontaneously formed on the GaN substrate through a heat treatment process for 300 +/- 30 seconds after the gold deposition step;
/ RTI >
In the GaN substrate preparation step,
Preparing a GaN wafer having 10 +/- 2 mu m-thick grown on a sapphire substrate having an off-axis of +/- 0.1 DEG; And
The GaN wafer is indium-bonded to the Inconel holder and is subjected to a cleaning process in a pulse laser deposition chamber at 650 to 750 ° C in a 1 × 10 -4 × (± 10%) Torr atmosphere for 0.5 to 1 hour; , Wherein:
In the gold deposition step,
The resulting GaN substrate was subjected to a growth at a growth rate of 0.05 ± 0.01 nms -1 in a plasma ion-coater chamber through which a 1 × 10 -1 × (± 10%) torr state and an ionization current of 3 to 5 mA flowed Is deposited,
A gold layer having a thickness of 4 ± 0.5 nm is deposited in the gold deposition step and an annealing temperature is controlled in a range of 400 to 800 ° C. in the growth step to form the shape, size, and density of the spontaneously formed gold nanoparticles And a control unit
The average height of the spontaneously formed gold nanoparticles is increased as the annealing temperature is increased to 750 ° C. in the growing step and the average height of the gold nanoparticles is decreased at the annealing temperature of 800 ° C. Wherein the control of the growth rate of the gold nanoparticles on the GaN layer is controlled by controlling the growth rate of the gold nanoparticles.
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