EE672 Microelectronics Lab

Report: RCA cleaning & Dry Oxidation

Abhijeet Darekar (24M1209)
 1. Explain the detailed procedure of RCA Cleaning.

Precautions:
 Use dedicated gloves before starting RCA cleaning procedure.
 Use Teflon lab ware for HF based chemicals.
RCA Cleaning Procedure
1. 2% HF Dip (Hydrofluoric Acid Dip) & DI water rinse

 2% HF solution is prepared by mixing 10ml of hydrofluoric acid (HF) to 240ml of DI

water.
 Submerge the silicon wafer in the 2% HF solution.
 Rinse the wafer with DI water to remove any native oxide layer from the wafer's
surface.

2. RCA 1 (Ammonium Hydroxide and Hydrogen Peroxide Cleaning)

 Prepare RCA 1 solution:
o Mix 180 ml of DI water.
o Add 25 ml of ammonium hydroxide (NH₄OH) to the DI water.
o Heat the mixture on a hot plate at 75°C for 5 minutes.
o Add 50 ml of hydrogen peroxide (H₂O₂) to the solution, load silicon wafer to this
solution and heat at 75°C for an additional 8 minutes
 After that allow the wafer to cool at room temperature for 12 minutes.
 Rinse the wafer with DI water.

3. HF Dip (After RCA 1)

 After RCA 1 cleaning, dip the wafer in a 2% HF solution again to remove any native
oxide.
 Rinse the wafer with DI water to ensure that no residue is left on the wafer surface.
4. RCA 2 (Hydrochloric Acid and Hydrogen Peroxide Cleaning)
 Prepare RCA 2 solution:
o Mix 180 ml of DI water.
o Add 25 ml of hydrochloric acid (HCl) to the DI water.
o Heat the mixture on a hot plate at 75°C for 5 minutes.
o Add 50 ml of hydrogen peroxide (H₂O₂) to the solution, load silicon wafer to this
solution and heat at 75°C for an additional 5 minutes
 After that allow the wafer to cool at room temperature for 12 minutes.
 Rinse the wafer thoroughly with DI water.
 RCA2 cleaning will remove any heavy metal contaminants and ionic impurities from the
wafer

5. HF Dip (After RCA 2)

 Dip the wafer in a 2% HF solution once again to remove any oxide layers that might
have formed.
 Rinse the wafer with DI water to ensure it is clean and free of chemicals.

6. Nitrogen Gas Drying

 After all cleaning steps are complete, dry the wafer by blowing nitrogen gas over the
surface to remove any residual water.
2. A new cleaning procedure has been proposed which is based on H2O saturated with
O2 as an oxidant. This has been suggested as a replacement for the H2O2 oxidizing
solution used in the RCA clean. Suppose a Si wafer, contaminated with trace amounts
of Au, Fe, and Cu is cleaned in the new H2O/O2 solution. Will this clean the wafer
effectively? Why or why not? Explain.

1. Cleaning Effectiveness for Metal Contaminants:

The trace metal contaminants you mentioned — Au (gold), Fe (iron), and Cu (copper) —
are typically inorganic in nature, and their removal requires a process capable of
dissolving or oxidizing them.

 Au (Gold):
o Gold is a noble metal, meaning it's highly resistant to oxidation and dissolution
under normal conditions. The H₂O/O₂ solution may not oxidize or dissolve gold
effectively.
 Fe (Iron) and Cu (Copper):
o Iron (Fe) and Copper (Cu) are less resistant to oxidation than gold and can be
oxidized to their respective oxides (e.g., Fe₂O₃ or CuO). Oxidation of these metals
could help in their removal, but the oxidation power of O₂ in water might be
limited at lower concentrations.
o While O₂ can oxidize metals like iron and copper to form oxides, the rate and
effectiveness of oxidation depend on various factors, including temperature,
concentration of oxygen, and the chemical environment. At room temperature
and with O₂ saturated in water, the oxidation rate may not be as rapid or
effective compared to the powerful oxidation provided by H₂O₂ in the traditional
RCA cleaning.

2. Role of H₂O/O₂ Solution:

 The H₂O/O₂ solution could theoretically provide some degree of oxidation to certain
contaminants, especially organic materials and potentially some metal oxides.
 However, O₂ in water is generally less reactive than H₂O₂ (hydrogen peroxide), which is
why H₂O₂ is commonly used in RCA cleaning. H₂O₂ is a strong oxidizing agent that
actively breaks down and oxidizes a wide range of contaminants, including organic
materials and metals, forming water-soluble compounds that can be rinsed away.

3. Comparison to RCA Cleaning with H₂O₂:

 The RCA cleaning process uses H₂O₂ as an oxidizing agent, which is very effective at
breaking down organic contaminants and helping to dissolve certain metals, especially
when combined with ammonium hydroxide (NH₄OH) for organic contamination removal.
  The H₂O/O₂ solution may not have the same level of oxidative power as H₂O₂, and thus,
it is likely to be less effective at cleaning metal contaminants like Au, Fe, and Cu
compared to the more aggressive H₂O₂ solution in the RCA clean.

3. Write the Dry Oxidation procedure. (Include checklists and precautions also if any).

Dry Oxidation Procedure

1. Pre-operation Checks:
 Ensure the water supply is available for cooling systems.
 Confirm that the power supply to the furnace is functioning correctly.
 Verify that the oxygen (O₂) and nitrogen (N₂) cylinders are properly set up and
functional. Ensure that the O₂ cylinder has adequate pressure.
2. Powering Up the Furnace:
 Turn on the Main Circuit Breaker (MCB) and the Furnace Main Power to start the
furnace.
 Open the N₂ gas gate valve to initiate nitrogen flow into the furnace.
3. Gas Flow Setup:
 Set the N₂ inflow to 2 divisions and the outflow to 0.5 divisions to establish a stable
nitrogen environment.
 Set the furnace’s initial temperature to 500°C across all zones.
4. Loading the Wafers:
 Once the furnace temperature reaches 500°C, it is ready for wafer loading.
 Wear the cleanroom gown before entering the cleanroom to prevent contamination.
 Open the furnace door and cap, then carefully load the wafers onto the wafer boat
inside the furnace chamber.
 Place the wafers with the shiny surface facing towards the flow (Micro-1) for optimal
oxidation.
 Position the wafer boat in the middle of the furnace for uniform heating.
 Close the furnace door and cap securely to avoid contamination and gas leaks.
5. Furnace Ramp-Up and Stabilization:
 After loading the wafers, remove the gown and return to the control area.
 Ramp up the furnace temperature to 1100°C for the oxidation process to take place.
 Wait for the temperature to stabilize at 1100°C across all zones.
6. Oxygen Gas Introduction:
  Once the temperature stabilizes, turn on the O₂ gas gate valve and set the oxygen flow
to 20 divisions.
 Turn off N₂ inflow after introducing oxygen to ensure that the oxidation process is driven
by O₂.
 Wait for 3 minutes to allow the oxygen to fully react and form the silicon dioxide layer
on the wafer surface.
7. End of Oxidation and Cooling:
 After the 3-minute waiting period, turn off the O₂ inflow to stop the oxidation process.
 Set the N₂ inflow back to 2 divisions to help maintain an inert environment during the
cooling process.
 Ramp down the furnace temperature to room temperature (RT), reducing it at a rate of
about 30°C/min to avoid thermal shock.
8. Furnace Shutdown and Wafer Unloading:
 Once the furnace temperature reaches 30°C across all zones, turn off the furnace
power.
 Turn off N₂ inflow and outflow, as well as the gas gate valves for both O₂ and N₂.
 Turn off the main MCB and the gas cylinders to stop the gas supply and power.
 Unload the wafers from the furnace once the chamber is safe to open.
 Remove the wafers from the wafer boat and place the boat back into the furnace.
 Close the furnace door securely after the process is complete.

Precautions:
 Do not touch the tips of hot surfaces inside the furnace. High temperatures can cause
severe burns or injury.
 Always use dedicated apparatus for the oxidation process to avoid cross-contamination
between different processes or chemicals.

4.What are the other ways to grow/deposit SiO2 on Si? Explain the CVD and Sputter
deposition methods for SiO2. What are the advantages and disadvantages? Mention the
applications of these (Sputter and CVD Process) oxide deposition methods (two
applications possible usage of the process in CMOS).
Here are the different methods to grow or deposit SiO₂ on silicon:
Thermal Oxidation
 Dry Oxidation
  Wet Oxidation
Chemical Vapor Deposition (CVD)
 Low Pressure CVD (LPCVD)
 Plasma-Enhanced CVD (PECVD)
 High-Density Plasma CVD (HDPCVD)
Sputter Deposition
 RF Sputtering
 DC Sputtering
Atomic Layer Deposition (ALD)
Spin Coating (using SiO₂ precursors like TEOS)
Evaporation (Physical Vapor Deposition - PVD)
Sol-Gel Process
Molecular Beam Deposition (MBD)
 Chemical Vapor Deposition (CVD) for SiO₂ Deposition
CVD is a process where a chemical reaction occurs in the vapor phase to form a solid film on a
substrate. In SiO₂ CVD, silicon dioxide is deposited onto a silicon wafer by introducing precursor
gases such as silane (SiH₄) or tetraethoxysilane (TEOS), along with an oxidizing gas like O₂ or O₃
into a reactor chamber. The precursors decompose at high temperatures (typically 300°C to
900°C) to form SiO₂ films.
CVD Process Steps:
1. Gaseous precursors (like SiH₄ or TEOS) are introduced into the deposition chamber.
2. Oxidizing gas (O₂) is added to facilitate the formation of SiO₂ from the silicon precursor.
3. Chemical reaction occurs at the surface of the silicon wafer, resulting in a SiO₂ film
formation.
4. The by-products of the reaction (e.g., SiH₄ decomposition products) are exhausted out
of the reactor.
Advantages of CVD for SiO₂:
1. Uniformity: Provides uniform oxide films over large areas, which is essential for
integrated circuits.
 2. Conformality: Able to deposit SiO₂ films over complex topographies, such as on trenches
or deep vias, which is particularly important for advanced CMOS devices.
3. Control over film properties: The process allows for good control over the thickness and
quality of the oxide layer.
4. Reproducibility: High reproducibility and consistency in film deposition.
Disadvantages of CVD for SiO₂:
1. High-temperature process: The process typically requires high temperatures, which may
limit its use for certain substrates or in low-temperature processes.
2. Complexity and cost: CVD equipment can be complex and expensive, especially for Low-
Pressure CVD (LPCVD) or Plasma-Enhanced CVD (PECVD) processes.
3. Film stress: The deposition process can introduce stress in the oxide layer, which might
affect the device performance or cause cracking if not properly controlled.
Applications of CVD in CMOS:
1. Gate Oxide Formation: CVD SiO₂ is used to form high-quality gate oxides in MOS
transistors.
2. Interlayer Dielectric: CVD SiO₂ can be used as an insulating layer between metal
interconnects in multi-level interconnection schemes (for example, intermetal dielectric
in advanced CMOS processes).

 Sputter Deposition for SiO₂ Deposition

Sputtering is a physical vapor deposition (PVD) technique in which atoms are ejected from a
solid target material (in this case, SiO₂) and deposited onto a substrate (like a silicon wafer). In
SiO₂ sputtering, an inert gas like argon (Ar) is used to bombard a SiO₂ target in a vacuum
chamber. This causes the SiO₂ target material to eject atoms, which then deposit on the wafer
to form a thin oxide film.
Sputter Deposition Process Steps:
1. Inert gas (argon) is introduced into the chamber, and a high voltage is applied to ionize
the gas.
2. Argon ions are accelerated towards a SiO₂ target, causing sputtering of SiO₂ atoms.
3. The ejected SiO₂ atoms travel towards the silicon wafer, where they are deposited as a
thin SiO₂ film.
Advantages of Sputtering for SiO₂:
 1. Lower deposition temperature: Sputtering can be done at lower temperatures
compared to CVD, making it more compatible with temperature-sensitive substrates.
2. Good step coverage: Sputtering provides relatively good step coverage, which is useful
for covering complex topographies.
3. Controlled composition: Since the sputtering target is a solid SiO₂ target, the
stoichiometry of the oxide film is inherently controlled.
Disadvantages of Sputtering for SiO₂:
1. Film quality and density: Sputtered SiO₂ films tend to be less dense and may have
higher porosity compared to films deposited by CVD.
2. Slower deposition rates: Sputtering typically has slower deposition rates compared to
CVD, which can increase process times.
3. Uneven film thickness: Sputtering can sometimes produce non-uniform film thickness
due to the line-of-sight nature of the process, though this can be mitigated by rotating
the wafer during deposition.
Applications of Sputtering in CMOS:
1. Passivation Layers: Sputtered SiO₂ is often used as a passivation layer in CMOS devices
to protect the underlying structures from contaminants and moisture.
2. Gate Oxides for Specific Applications: In some specialized CMOS processes, sputtered
SiO₂ can be used for gate oxide layers, particularly when low-temperature processing is
required.