JP6519792B2 - Method of manufacturing hydrogenated diamond MISFET having normally-off characteristics - Google Patents

Description

  The present invention relates to a method of manufacturing a hydrogenated diamond MISFET having normally-off characteristics, and more particularly to a method of normally-off making a MISFET of this type which has normally-on characteristics as it is.

  Wide band gap semiconductors such as GaN, SiC, and diamond have high band gap energy, high carrier mobility, and high breakdown electric field (Non-patent documents 1 to 5), making high power and high frequency electronic devices It is well known that it is suitable for According to theoretical calculations with figure of merit (NPLs 6 and 7), diamond based power devices have much higher output power and much lower power loss compared to GaN and SiC based devices Indicates Therefore, diamond is considered as a strong candidate for the next generation of power devices (Non-Patent Document 8).

Hydrogenated diamond (H-diamond) epitaxial layers accumulate holes with a sheet hole density of 10 ¹⁴ cm ^-2 on the surface (9, 10), so hydrogenated diamond is a high performance diamond-based electronic device. It is considered as a suitable p-type channel layer for preparation (nonpatent literature 11-14). The mechanism of hole formation is still under discussion, but both carbon-hydrogen (C-H) bonds and surface adsorbate acceptors are essential for the formation of hole accumulation. It is believed that the conditions are as follows (Non-Patent Documents 15 and 16). In order to control such high density carriers (about 10 ¹⁴ cm ^-2 ), a metal-insulator-semiconductor (MIS) gate structure using an insulator having a high dielectric constant is required (non-patent document) 17). In addition to this, it is important to prepare a depletion (D) mode and an enhancement (E) mode MIS field effect transistor (MISFET) corresponding to the normally on operation and the normally off operation, respectively.

Recently, in order to achieve this purpose, a high dielectric constant (high-k) insulator has been deposited on hydrogenated diamond to produce a MISFET (Non-Patent Documents 18 to 21). A two-layer high dielectric constant oxide insulator was fabricated by atomic layer deposition (ALD) and radio frequency sputter deposition (SD). A thin ALD insulator about 4.0 nm thick served to keep the hydrogen surface from sustaining discharge damage during SD insulator deposition. According to the present inventor previously reported (non-patent documents 18 to 21), SD-Ta ₂ O ₅ / ALD-Al ₂ O ₃ / hydrogenated diamond and SD-ZrO ₂ / ALD-Al ₂ O ₃ The hydrogenated diamond MISFET exhibited normally on characteristics (Non-patent Documents 18 and 19). As _{Conversely, SD-LaAlO 3 / ALD-} Al 2 O 3 / hydrogenated diamond and AD-HfO ₂ / hydrogenation diamond MISFET showed normally-off characteristic (non-patent literature 20, 21). This is believed to be the first report showing that E-mode MISFET can be produced, and proposed development of a method for producing a hydrogenated diamond based inverter (Non-patent Document 22), but E-mode MISFET The reason for becoming normally-off properties was also unclear as to which particular processing step in the manufacturing process resulted in normally-off properties.

  It is an object of the present invention to clarify conditions for producing a normally-off hydrogenated diamond MISFET and to enable a normally-off / on hydrogenated diamond MISFET to be separately fabricated.

According to one aspect of the present invention, there is provided a method of producing a hydrogenated diamond MISFET using a multi-layered gate oxide, wherein the gate oxide is formed at 160 ° C. at any time after formation on the hydrogenated diamond. A method of making a hydrogenated diamond MISFET with normally-off characteristics is provided that includes the step of annealing in the range of 350 ° C.
Here, the multi-layered gate oxide is formed of a first layer formed of an atomic deposition layer adjacent to the hydrogenated diamond and a second layer formed by sputtering on the first layer. May be included.
Further, the first layer is formed of a material selected from the group consisting of Al ₂ O ₃ and HfO _2, and the _second layer is selected from LaAlO ₃ , Ta ₂ O ₅ , ZrO ₂ , HfO ₂ It may be formed of a material.
The hydrogenated diamond may be an epitaxially grown layer.

  According to the present invention, the hydrogenated diamond MISFET can be made normally off by simple processing without substantial deterioration in performance.

The figure which shows the outline of the manufacturing process of hydrogenation diamond MISFET. The schematic diagram of the cross-section of the hydrogenation diamond MISFET manufactured by the Example of this invention. It shows the _I DS _{-V DS} characteristics of hydrogenated diamond MISFET manufactured in an embodiment of the present invention. FIG. 7 shows the transfer characteristics of the hydrogenated diamond MISFET manufactured according to an embodiment of the present invention. STEM image of the LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond interface of a hydrogenated diamond MISFET manufactured according to an embodiment of the present invention. (A) STEM image before annealing. (B) STEM image after annealing. Shows C, La, O and Al elements in the depth direction profile of the at LaAlO ₃ / _Al 2 _{O 3} / hydrogenation diamond interface hydrogenated diamond MISFET manufactured in an embodiment of the present invention. (A) Profile before annealing. (B) Profile after annealing at 180 ° C. It shows the C-V characteristics of the LaAlO ₃ / _Al 2 _{O 3} / hydrogenated diamond MIS capacitor. The inset is a top view of the planar MIS capacitor. FIG. 8 (a) shows the schematic structure and band diagram for the hydrogenated diamond epitaxial layer, and FIGS. 8 (b) and (c) and (d) show LaAlO ₃ / Al ₂ O ₃ / before and after annealing, respectively. Figure 1 shows a schematic structure and band diagram for hydrogenated diamond.

  According to the inventor's previous studies, whether a hydrogenated diamond based MISFET is normally on or normally off is independent of the insulating material and device structure, but in the manufacturing process It was found to be highly reproducible (18-21). This will be described with reference to FIG. The mesa structure fabrication in step 1 is the first step common to both D-mode and E-mode MISFETs, but the second step is different. In the case of the E mode (normally off) MISFET, gate oxide and contact were formed in step 2. On the other hand, in the case of the D mode (normally on) MISFET, a source / drain ohmic contact was produced in step 2. After publishing this research result, the inventors proceeded further research and compared the experimental details between the two fabrication processes, and as a result, the obvious difference between the insulator / hydrogenated diamond of normally-off MISFET It was found that the interface was annealed at 180 ° C. for 5 minutes during photoresist baking, while the annealing process was not performed for the insulator / hydrogenated diamond interface of a normally on MISFET. Since the hydrogenated diamond channel layer is sensitive to heat (Non-patent Document 23), it is believed that holes disappear by the annealing step and a normally-off characteristic is obtained. Accordingly, the present invention utilizes the effect of the annealing process on the electrical properties of the hydrogenated diamond based MISFET.

According to one aspect of the invention, the normally on / off operation of a hydrogenated diamond based MISFET, such as, for example, LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond MISFET, can be controlled by annealing at 180 ° C. By performing this _annealing, the value of _{V TH} of LaAlO ₃ / _Al 2 _O 3 / hydrogenation diamond MISFET has been changed to -0.5 ± 0.1 V from 0.8 ± 0.1 V, this is MISFET Indicates a change from normally on operation to normally off operation. Moreover, the flat band voltage of the CV curve changed from zero to a negative value by performing this annealing. The annealing temperature at which the hydrogenated diamond MISFET can be changed from the normally on operation to the normally off operation is in the range of 160 ° C to 350 ° C.

  The mechanism of normally on / off control is interpreted as follows. Before annealing, the adsorbate acceptor on the hydrogenated diamond channel layer results in hole accumulation in the hydrogenated diamond channel layer, whereby the MISFET exhibits normally on characteristics. However, after annealing in the temperature range described above, the adsorbate acceptor diffuses therefrom and dissipates, or is offset by the positive charge in the oxide. This causes a significant reduction in the hole density in the hydrogenated diamond channel layer and causes the MISFET to exhibit normally-off characteristics. By controllably forming hydrogenated diamond based MISFETs of normally on / normal off characteristics, it becomes possible to develop CMOS integrated circuits that require normally off characteristics.

  Hereinafter, the present invention will be described in more detail by way of examples. However, needless to say, it should be noted that the present invention is not limited to the following examples.

A hydrogenated diamond epitaxial layer was grown on a 2.5 × 2.5 × 0.5 mm ³ size single crystal diamond (001) substrate by microwave plasma-enhanced chemical vapor deposition (CVD) technique. The deposition temperature, chamber pressure, CH ₄ flow rate and H ₂ flow rate during this CVD process were 900 to 940 ° C., 80 Torr, 0.5 sccm and 500 sccm, respectively. A hydrogenated diamond MISFET was fabricated on the hydrogenated diamond epitaxial layer by the process shown in FIG. The process for producing such a hydrogenated diamond MISFET is itself well known to those skilled in the art, so a detailed description will not be given here, but if necessary, please refer to Non-Patent Document 19.

In order to investigate the influence of annealing on the electrical properties of the MISFET, initially, a normally on mode MISFET was fabricated using the process shown in FIG. After fabricating this MISFET, it was annealed at 180 ° C. for 5 minutes and 10 minutes. Here, the two-layer insulator of the MISFET was an ALD-Al ₂ O ₃ buffer layer and an SD-LaAlO ₃ layer deposited sequentially on hydrogenated diamond at 120 ° C. and room temperature, respectively. For the specific conditions of the ALD method and the SD method, refer to Non-Patent Document 20.

A schematic view of the cross-sectional structure of the produced MISFET is shown in FIG. Here, the thicknesses of the ALD insulator (ALD-Al ₂ O ₃ buffer) layer and the SD insulator (SD-LaAlO ₃ ) layer were 3.0 nm and 23.4 nm, respectively. These thicknesses were confirmed by ellipsometer. The layer configuration of each of the gate electrode, the source electrode and the drain electrode was Au (200 nm) / T (20 nm) / Pd (10 nm), and vapor deposition was performed by electron beam evaporation. Here, Pd is a metal contact to the hydrogenated diamond surface. The gate length (L _G ) and the gate width (W _G ) of the MISFET were maintained at 4 μm and 150 μm, respectively. The distance between the source / drain ohmic connection and the oxide insulator (dS _{/ D-oxide} ) was maintained at 5 μm. A planar type MIS capacitor was manufactured simultaneously with the MISFET. The diameter of the circular gate electrode was 200 μm, and the distance between the ohmic Au / Ti / Pd contact and the oxide insulator was 10 μm. The electrical properties of these MISFETs and MIS capacitors before and after annealing were measured at room temperature using a high performance MX-200 / B prober. The frequency for measuring the capacitance-voltage characteristics of the MIS capacitor was maintained at 50 kHz. Atomic resolution scanning transmission electron microscopy (STEM) with Cs collector and energy dispersive x-ray analysis (EDX) system to analyze the chemical structure of LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond interface )It was used.

FIG. 3 shows the drain-source current-voltage (I _DS -V _DS ) characteristics of the LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond MISFET before and after annealing at 180 ° C. FIG. 3 (a) shows the I _DS -V _DS characteristics before annealing, FIG. 3 (b) after annealing for 5 minutes, and FIG. 3 (c) after annealing for 10 minutes. Here, the gate-source voltage was changed from +5.0 V to 2.5 V, in +0.5 V steps. Each of these MISFETs operated well and exhibited p-type channel characteristics. For any I _DS- V _DS curve, a clearly linear region is observed in the low V _DS range. This indicates that the Au / Ti / Pd metal and the hydrogenated diamond surface have a good ohmic connection. The maximum value of the _{I DS} in the case of pre-anneal _{MISFET (I DS maximum) (I} DSmax) was -31.3mA · ^{mm -1.} The I _DSmax when annealed at 180 ° C. for 5 minutes and 10 minutes was −28.3 mA · mm ⁻¹ and −28.7 mA · mm ⁻¹ , respectively.

The transfer characteristics of this MISFET before and after annealing are shown in FIG. The threshold voltage (V _TH ) can be determined from the relationship between −√ (| I _DS |) and V _GS . _{V TH} before annealing has been determined to 0.8 ± 0.1 V, which shows the normally-on characteristics. However, the _{V TH} after annealing of 5 minutes and 10 minutes at 180 ° C. varies with -0.5 ± 0.1 V, was the normally-off characteristics. From the relationship between V _TH and the effective mobility (μ _eff ) (non-patent document 21), the values of μ _eff before and 5 minutes after annealing at 180 ° C. for 5 minutes and 10 minutes are 56.5 ± 0.5 cm, respectively. It was calculated as ² · V ⁻¹ · s ⁻¹ , 57.7 ± 0.5 cm ² · V ⁻¹ · s ⁻¹ and 58.2 ± 0.5 cm ² · V ⁻¹ · s ⁻¹ . Note that the value of μ _eff is almost constant for both D mode and E mode MISFETs. This indicates that the annealing does not degrade the MIS interface. The post-annealing can change the MISFET from the normally on characteristic to the normally off characteristic. This indicates that the equilibrated holes in the hydrogenated diamond channel layer (NPL 24) disappear when annealed at 180 ° C.

In order to further clarify the effect of annealing to the insulator / hydrogenated diamond interface, STEM images of the LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond structure and the CV characteristics of the MIS capacitor were investigated.

FIG. 5 is a STEM image of the LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond interface, and FIG. 5 (a) shows the image before annealing and FIG. 5 (b) shows the image after annealing. By comparing the STEM images before and after annealing, it can be seen that the annealing does not change either the steepness of the oxide / hydrogenated diamond interface or the amorphous structure of the oxide insulator. Therefore, annealing at a low temperature of 180 ° C. can not affect the crystal structure of the diamond interface.

FIG. 6 is a depth direction profile of C, La, O and Al elements at the LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond interface, and FIG. 6 (a) is before annealing, FIG. 6 (b) is 180 The profile after annealing in ° C is shown. It can be seen from FIG. 6 (a) before annealing that the La, Al and O elements are uniformly distributed. However, the profile after annealing shown in FIG. 6 (b) indicates that the distributions of La and Al elements are not uniform.

FIG. 7 shows the C-V characteristics of the LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond MIS capacitor. The inset at the bottom left of FIG. 7 is a top view of the planar MIS capacitor. All of the C-V curves in the figure have a well-defined accumulation region and a depletion region. This suggests that high quality LaAlO ₃ / Al ₂ O ₃ insulators are fabricated on hydrogenated diamond. The C-V curves prior to annealing in the depleted region and after annealing for 5 minutes at 180 ° C. show a sharp dependence on the gate bias, which corresponds to the LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond interface. Low-density interface state in the above (Non-Patent Documents 26 and 27). When the annealing time is 10 minutes, the depleted C-V curve is a curve which spreads slightly to the side. This probably indicates that the quality of the LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond interface has been deteriorated by long-time annealing (Non-patent Documents 26 and 27). An important feature is that a 0.47 V voltage shift (V _Shift ) occurs in the CV curve before and after annealing. The flat band voltage V _FB = V _GS = 0 before annealing as indicated by a thick arrow pointing downward at the position of gate bias = 0 V in FIG. 7 shifts by −0.47 V after annealing at 180 ° C. This means that the annealing reduces the negative charge density at the ALD-Al ₂ O ₃ / hydrogenated diamond interface and the sheet hole density N _{p in the} hydrogenated diamond channel layer. N _p can be evaluated by the following equation.

N _p = C _OX (V _shift / q) (1)

Here, q and C _OX are an elementary charge (1.6 × 10 ⁻¹⁹ C) and a capacitance (0.29 μF · cm ⁻² ) of the LaAlO ₃ / Al ₂ O ₃ insulator, respectively. From this, the value of N _p can be calculated to be 8.5 × 10 ¹¹ cm ⁻² .

The table below summarizes the effects of annealing on the normally on / off characteristics of hydrogenated diamond MISFETs using various oxide insulators and adopting various device structures (sizes) It is. Here, that the rightmost column is On or Off indicates that the MISFET has a normally on characteristic and a normally off characteristic, respectively. In addition, the gate width W _G was 150 μm for all the MISFETs. The data in the table includes the data described in the papers (non-patent documents 18 to 21) previously published by the inventor of the present application.

In the LaAlO ₃ / Al ₂ O ₃ / hydrogenated diamond MISFET, V _TH takes a positive value corresponding to a normally on characteristic if there is no annealing step during the manufacturing process. Conversely, if the annealing step is present during the manufacturing process, V _TH is a negative value corresponding to the normally-off characteristics. In Non-Patent Documents 18, 19 and 21 in the present inventor's article referred to above, SD-Ta ₂ O ₅ / ALD-Al ₂ O ₃ / hydrogenated diamond, AD-ZrO ₂ / ALD-Al ₂ With regard to O ₃ / Hydrogenated diamond and SD-HfO ₂ / ALD-HfO ₂ / Hydrogenated diamond MISFET, only V _TH with or without annealing was examined, but these are also SD- It shows normally on / off characteristics consistent with the conclusions obtained from LaAlO ₃ / ALD-Al ₂ O ₃ / hydrogenated diamond MISFETs. After annealing the MISFET at 180 ° C., the hole density of the hydrogenated diamond channel layer can be considered to be greatly reduced. As surface CH bonds and adsorbate acceptors are required for hole accumulation in the equilibrium stage of V _GS = 0 (Non-patent documents 15 and 16), decomposition of CH bonds or disappearance of adsorber acceptors It is believed that the result is a normally-off feature. However, the C—H bond is reported to be very stable when the annealing temperature is 200 ° C. or less (Non-patent Document 23). Therefore, the phenomenon that is considered to be actually occurring is a decrease in the adsorbant acceptor density in the portion near the oxide / hydrogenated diamond interface in the oxide. This will be explained in more detail below.

FIG. 8 (a) shows the schematic structure and band diagram for the hydrogenated diamond epitaxial layer, and FIGS. 8 (b) and (c) and (d) show LaAlO ₃ / Al ₂ O ₃ / before and after annealing, respectively. 1 shows a schematic structure and band diagram for hydrogenated diamond. VBM, CBM and EF in FIG. 8 indicate valence band maximum, conduction band minimum and Fermi level, respectively.

In the case of the hydrogenated diamond epitaxial layer shown in FIG. 8 (a), a negatively charged acceptor is present on the C—H bond near the surface (Non-Patent Document 23), and the transfer doping architecture (transfer doping architecture) As a result, holes (h ^{+ in} FIGS. 8A and 8B) are accumulated in the hydrogenated diamond channel layer (Non-patent Documents 15 and 28). Here, the hole density is equal to the density of negatively charged acceptors. Hydrogenated diamond exhibits band bending upward toward the surface (Non-patent Documents 25 and 29). This means hole accumulation.

After depositing the LaAlO ₃ / Al ₂ O ₃ double layer on hydrogenated diamond, the negatively charged acceptor is held close to the insulator as shown in FIG. The diamond exhibits an upward band bend towards the ALD-Al ₂ O ₃ / hydrogenated diamond interface. Since both C—H bonds and negatively charged acceptors are located at the interface, holes can be accumulated in the hydrogenated diamond channel layer, and thus the MISFET before annealing exhibits normally on characteristics. After annealing the MISFET at 180 ° C., two changes can occur at the interface. One of them is the absence of negatively charged acceptors at the interface as shown in FIG. 8 (c). In this case, the energy band of the hydrogenated diamond is flat or shows a downward curve to the interface. On the other hand, as shown in FIG. 8 (d), negatively charged acceptors still exist at the interface, and the energy band of hydrogenated diamond shows a slight upward bend to the interface. However, after annealing, negatively charged acceptors are offset by the positive charge generated in the LaAlO ₃ / Al ₂ O ₃ mixed layer. In either of the two possible interface charge states described above, it is difficult for holes to be accumulated in the hydrogenated diamond channel layer at G _GS = 0. Thus, the annealed MISFET exhibits normally-off characteristics.

Therefore, it is believed that the cause of the normally-off characteristic is a decrease in acceptor density near the insulator / hydrogenated diamond interface after annealing. However, it is difficult at present to clarify the hole transfer mechanism for the normally-off MISFET. Holes are probably derived from surface channels where the hydrogenated diamond is not covered with oxide insulator or remaining acceptors in the diamond epitaxial layer (31). Another possible explanation is that the negative V _GS changes the balance between the negatively charged acceptor and the positive charge offsetting it, leading to hole accumulation.

Among the negatively charged adsorbates that can be used are anions containing oxygen such as HCO ₃ ⁻ and OH ⁻ . Annealing at the above mentioned annealing temperature range, for example 180 ° C., results in adsorbate loss or formation of a positively charged charge compensator. Since it is reported that hydrogenated diamond MISFET with a gate of only Al ₂ O ₃ showed thermally stable normally on mode operation (non-patent documents 32, 33), the normally off characteristic by annealing is SD This is considered to be a feature obtained only with a hydrogenated diamond MISFET having an ALD / ALD bilayer insulator gate. On the other hand, the electrical characteristics of the MISFET annealed at a temperature higher than 180 ° C. were also examined. It was found that the MISFET after annealing at 300 ° C. operates well with normally-off characteristics. Also, the MISFET annealed at 400 ° C. did not operate well. The upper limit of the annealing temperature for making the hydrogenated diamond MISFET normally off can be practically raised to 350.degree.

Dissociation of acceptors or formation of counterbalances is probably due to the metallurgical reaction between the LaAlO ₃ layer and the Al ₂ O ₃ layer after annealing. This was confirmed by EDX analysis shown in FIG. In addition to this, the observation of the STEM image shown in FIG. 5 showed that this reaction did not degrade the interface. This conclusion is supported by the almost identical values of I _DSmax and μ _eff before and after annealing. Recently, the inventor has discovered a thin amorphous interfacial layer in a single crystal AlN layer grown by metal-organic vapor phase epitaxy on hydrogenated diamond. This thin amorphous layer was also observed at the polycrystalline AlN / hydrogenated diamond interface (34). Thus, presumably, the presence of thin layers on the nanometer scale affects the general behavior of the interface between the oxide or nitride and the hydrogenated diamond.

  As described above, according to the present invention, a normally-off characteristic MISFET generally used in semiconductor devices such as Si can be easily created by the addition of a simple process. It is considered to contribute greatly to the practical application of devices using diamond.

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Claims (3)

In the production method of a hydrogenated diamond MISFET using Gate oxide, wherein each formed by hydrogenation diamond on the atomic layer deposition (ALD) and RF sputtering deposition _{(SD), SD-LaAlO 3} / ALD-Al _A bilayer selected from the group consisting of ₂ O ₃ , SD-Ta ₂ O ₅ / ALD-Al ₂ O ₃ , SD-ZrO ₂ / ALD-Al ₂ O ₃ , and SD-HfO ₂ / ALD-HfO ₂ A method of manufacturing a hydrogenated diamond MISFET having normally-off characteristics, comprising the steps of forming the gate oxide of structure and annealing at 180 ° C. The manufacturing method according to claim 1, wherein the annealing step anneals the hydrogenated diamond MISFET using the gate oxide for 5 minutes to 10 minutes . The hydrogenation diamond is a layer epitaxially grown method according to claim 1 or 2.