TWI633571B - Inductively coupled plasma processing chamber and corrosionresistant insulating window thereof and manufacturing method thereof - Google Patents

Abstract

The invention provides an inductively coupled plasma processing chamber and a corrosion resistant insulating window thereof, and a manufacturing method thereof, wherein the insulating window is coated with corrosion resistance on a plasma-facing side thereof by plasma enhanced physical vapor deposition The coating, the insulating window coated with the anti-corrosion coating, is subjected to a heat treatment step. Wherein the heat treatment step comprises a thermal annealing step. The anti-corrosion layer produced by the invention has high thickness, uniform texture, stable structure, low stress and no cracking.

Description

Inductively coupled plasma processing chamber and corrosion resistant insulating window thereof and manufacturing method thereof

The present invention relates to the field of semiconductor manufacturing, and in particular to an inductively coupled plasma processing chamber and a corrosion resistant insulating window thereof and a manufacturing method thereof.

The plasma processing chamber processes the substrate of the semiconductor substrate and the plasma plate using the working principle of the vacuum reaction chamber. The working principle of the vacuum reaction chamber is to pass a reaction gas containing a suitable etchant source gas into the vacuum reaction chamber, and then input RF energy to the vacuum reaction chamber to start the reaction gas to excite and maintain the plasma. The semiconductor substrate and the plasma plate are processed by etching a material layer on the surface of the substrate or depositing a material layer on the surface of the substrate.

Due to the presence of plasma in the plasma processing chamber, the components or walls of the plasma processing chamber exposed to the plasma are subject to varying degrees of corrosion. Different mechanisms for manufacturing corrosion resistant components have also been proposed in the industry.

How to manufacture stable and reliable anti-corrosion components is a goal developed by those skilled in the art.

In view of the above problems in the background art, the present invention proposes an inductively coupled plasma processing chamber and a corrosion resistant insulating window thereof and a manufacturing method thereof.

The first aspect of the invention provides a corrosion-resistant inductively coupled plasma An insulating window of the processing chamber, wherein: the insulating window is coated with an anti-corrosion coating on the side facing the plasma by enhanced physical or chemical vapor deposition, the insulating window coated with the anti-corrosion coating A heat treatment step was performed.

Further, the heat treatment step includes a thermal annealing treatment.

Further, the material of the anti-corrosion layer coating layer includes any one or more of the following: Y ₂ O ₃ , YF ₃ , ErO ₂ , Al ₂ O ₃ , SiC, AlN, ZrO ₂ .

Further, the anti-corrosion coating has a thickness greater than 40 um.

Further, the anti-corrosion layer coating has a multilayer structure.

Further, the ceramic substrate of the insulating window is quartz or aluminum oxide.

A second aspect of the present invention provides a method of fabricating an insulating window of an anti-corrosion inductively coupled plasma processing chamber, wherein the manufacturing method includes the steps of: providing an insulating window substrate; utilizing the insulating window substrate The enhanced physical or chemical vapor deposition is coated with a layer of corrosion resistant coating on its plasma facing side; the heat treatment step is then performed on the insulating window coated with the corrosion resistant coating.

Further, the heat treatment step includes a thermal annealing treatment.

Further, the manufacturing method further includes the steps of: roughening a side of the insulating window exposed to the plasma, and then using the enhanced physical or chemical vapor deposition on the insulating window substrate to face the plasma One side is coated with a corrosion resistant coating.

Further, the roughening treatment causes the surface roughness of the insulating window to be less than 0.5 um.

Further, the roughening treatment causes the surface roughness of the insulating window to be greater than 2 um.

Further, when the anti-corrosion coating has a multi-layered structure, the manufacturing method further includes the step of: performing a thermal annealing treatment step on the insulating window coated with the anti-corrosion coating, and then applying a plurality of layers on the insulating window The structural anti-corrosion coating is surface polished or ground.

Further, the temperature at which the corrosion-resistant coating is made by enhanced physical or chemical vapor deposition ranges from above room temperature.

Further, the anti-corrosion coating has a thickness greater than 40 um.

Further, when the corrosion-resistant coating has a multilayer structure, the thickness of each of the single-layer structures in the multilayer structure ranges from 0.1 um to 30 um, and the number of the multilayer structures can reach 1 to 100 layers.

According to a specific embodiment of the present invention, the corrosion-resistant coating deposited by the enhanced physical or chemical vapor deposition of the present invention has a relatively high thickness, and a thermal annealing step is performed on the insulating window to stabilize the coated insulating window. Structural stability. Due to the different materials and the formation of corrosion-resistant coatings by ion bombardment using enhanced physical or chemical vapor deposition, the corrosion-resistant coating applied to the insulating window necessarily has residual stress.

104‧‧‧Insulated window

104a‧‧‧Insulated window surface

200‧‧‧ Plasma processing chamber

202‧‧‧Metal sidewall

204‧‧‧Insulated window

204a‧‧‧One side of the plasma

206‧‧‧Base

208‧‧‧RF power supply

210‧‧‧RF coil

212‧‧‧ gas injection port

214‧‧‧RF source

820‧‧‧ source material

825‧‧‧Electronic gun

830‧‧‧electron beam

D2‧‧‧Anti-corrosion layer

D11‧‧‧Anti-corrosion coating

S21‧‧‧X-ray

S22‧‧‧Diffraction light

W‧‧‧ substrates

p‧‧‧Process area

A‧‧‧ hole

Fig. 1 is a schematic view showing the structure of an inductively coupled plasma processing chamber.

Fig. 2a is a schematic cross-sectional view showing the surface coating of the insulating window of the inductively coupled plasma processing chamber of the prior art by plasma spraying.

Figure 2b is a schematic cross-sectional view showing the surface coating of the insulating window of the inductively coupled plasma processing chamber of the prior art by directly doping the yttrium oxide with the bulk ceramic.

3 is a cross-sectional structural view showing an insulating window of an anti-corrosion inductively coupled plasma processing chamber according to an embodiment of the present invention.

4 is a flow chart showing the steps of a method for fabricating an insulating window of a corrosion-resistant inductively coupled plasma processing chamber according to an embodiment of the present invention.

Figure 5 is a schematic diagram showing the principle of a PEPVD for manufacturing a corrosion-resistant inductively coupled plasma processing chamber according to an embodiment of the present invention.

Figure 6 is a schematic diagram showing the principle of a thermal annealing step of a method for fabricating an insulating window of a corrosion-resistant inductively coupled plasma processing chamber according to an embodiment of the present invention.

Figure 7 is a list of parameters of a thermal annealing step of a method for fabricating an insulating window of a corrosion-resistant inductively coupled plasma processing chamber for different material layers in accordance with an embodiment of the present invention.

Figure 8 is a schematic diagram of the principle of Prague.

Fig. 9 is a graph for analyzing the effects of the present invention by performing a straight line fitting using the Bragg principle to obtain a slope.

Specific embodiments of the present invention will be described below with reference to the accompanying drawings.

It is to be noted that the terms "semiconductor process", "wafer" and "substrate" will be used interchangeably in the following description. In the present invention, they all refer to process parts that are processed in the processing chamber. The process member is not limited to a wafer, a substrate, a substrate, a large-area flat substrate, or the like. For convenience of description, the "substrate" will be mainly exemplified in the description and illustration of the embodiments herein.

The invention is applicable to all plasma processing chambers susceptible to plasma corrosion, including capacitively coupled plasma processing chambers (CCP) and capacitively coupled plasma processing chambers (ICP). For example, a gas shower head of a capacitively coupled plasma processing chamber, and various chamber sidewall top plates and the like. The insulating window of the capacitively coupled plasma processing chamber will be described below as an example. It should be noted that although the insulating window of the capacitively coupled plasma processing chamber will be described as an example, it cannot be used to limit the present invention, and the scope of application of the present invention is not limited thereto.

1 is a schematic block diagram of an inductively coupled plasma processing chamber in accordance with an embodiment of the present invention. FIG. 2 illustrates a plasma processing chamber 200 in accordance with one embodiment of the present invention. It should be understood that the inductively coupled plasma processing chamber 200 therein is merely exemplary, and the 200 may actually include fewer or additional components, and the arrangement of the components may also differ from that shown in FIG.

Figure 1 shows a cross-sectional view of an inductively coupled plasma processing chamber in accordance with a first embodiment of the present invention. The inductively coupled plasma processing chamber 200 includes a metal sidewall 202 and an insulating window 204 that form a hermetic vacuum enclosure and is evacuated by an evacuation pump (not shown). The insulating window 204 is by way of example only, and other top plate patterns may be used, such as dome-shaped, metal top plates with insulating material windows, and the like. The susceptor 206 includes an electrostatic chuck (not shown) on which the substrate W to be processed is placed. Bias power is applied to the electrostatic chuck to create a clamping force on the substrate W. The RF power of the RF power source 208 is applied to a RF power transmitting device located on the insulating window 204. In the embodiment, the radio frequency transmitting device includes a radio frequency coil 210. The processing gas is supplied from the gas source through the pipeline to the reaction chamber to ignite and sustain the plasma, thereby processing the substrate W. Preferably, the process gas The body enters the chamber from the gas injection port 212.

Referring to FIG. 1, it can be seen that the back surface of the insulating window 204 is directly exposed to the process region P and is under the corrosion of plasma in the process region P for a long time. Therefore, the prior art also employs many anti-corrosion mechanisms to solve this problem, but also brings new problems. For example, an insulating window 204 made of alumina Al ₂ O ₃ causes Al metal contamination, which is a taboo in the plasma processing chamber, and the insulating window 204 is located directly above the substrate W if the metal is contaminated from the insulating window. Dropping 204 on the substrate W will cause irreversible damage to the substrate. Insulated windows made of quartz often have a short life.

In order to create a stable and reliable insulating window, engineers have used a number of different methods to fabricate an inductively coupled plasma-insulated window with a corrosion resistant layer. Figure 2a is a schematic cross-sectional view showing the surface coating of the insulating window of the prior art inductively coupled plasma processing chamber by plasma spraying. As shown in Fig. 2a, the anticorrosive coating d11 coated on the surface 104a of the insulating window 104 by plasma spraying is formed by the use of sprayed cerium oxide particles, has a soft texture, and has a porous porous structure. As shown in FIG. 2, there are many holes a therein. Corrosion-resistant coatings d11 produced by plasma spray generally result in coatings having a high surface roughness (Ra greater than 4 microns or more) and correspondingly high porosity (volume ratios greater than 3%) in plasma It is easy to produce particle pollution in the body environment. In addition, since the hole a contains other gases, such as nitrogen gas, the purity of the anti-corrosion material of the anti-corrosion layer d11 is greatly reduced. When the anti-corrosion layer d11 is gradually thinned due to the corrosive action, the gas in the hole a is gradually released. It will also become an impurity gas in the substrate process. Therefore, the insulating window anti-corrosion layer d11 manufactured by the prior art using the plasma spraying method has a high roughness and a porous structure, so that the insulating window 104 or the anti-corrosion layer is liable to generate particles, which may cause Process substrate contamination. In addition, since the plasma sprayed layer in the gas injection hole is very rough and has weak adhesion to the substrate of the insulating window 104, when the sprayed gas shower head is used in the plasma processing chamber, The particles will come out of the gas injection port and fall onto the substrate.

Figure 2b is a schematic cross-sectional view showing the surface coating of the insulating window of the inductively coupled plasma processing chamber of the prior art using a bulk ceramic directly doped yttrium oxide method, which is directly doped with cerium oxide by a bulk ceramic. The material is used to fabricate the insulating window 104, but the insulating window 104 thus fabricated is poor in thermal shock resistance and there is a greater risk of cracking failure. As shown in Fig. 2b, the insulating window 104 thus manufactured still has a large number of holes a.

In addition, engineers use many other methods to create insulating windows, such as bulk yttria-based ceramic solid solutions or multi-phase ceramics, but at a very high manufacturing cost. For example, the insulating window of the composite structural ceramic, such as the sintered ceramic window with alumina and yttria double-layer powder, is complicated to process and high in cost.

In order to address the above-discussed drawbacks, the present invention provides an insulating window 204 of a corrosion-resistant inductively coupled plasma processing chamber 200 to improve the performance of the inductively coupled plasma processing chamber 200 fabricated by alumina. 3 is a cross-sectional view of an insulating window of an inductively coupled plasma processing chamber and a corrosion resistant coating thereof, using plasma enhanced physical or chemical vapor deposition (PEPVD or PECVD) in accordance with an embodiment of the present invention. The process deposits a thick and dense anti-corrosion coating d2 on the plasma side 204a over the insulating window 204, and then heat-treats the insulating window 204 coated with the anti-corrosion coating.

According to a preferred embodiment of the invention, the heat treatment step comprises a thermal annealing treatment. Corrosion-resistant coatings for enhanced physical or chemical vapor deposition can be achieved Thickness, but the stability of the structure in the anti-corrosion coating is poor, the crystal bond between the atoms is defective, and the stress is high. Such anti-corrosion coating is easy to crack, and the cracked anti-corrosion layer is easy to be in the process. The process is bombarded with a plasma to fall into the chamber to become particulate contamination or metal contamination, and even falls on the substrate W to cause the substrate W to be scrapped. The thermal annealing step enables the atoms in the anti-corrosion coating to vibrate with each other, filling the interatomic voids and making them more closely bonded to each other. The corrosion-resistant layer produced by the present invention using enhanced physical or chemical vapor deposition has a thick thickness and is structurally free of voids, and has a well-densified atomic structure or an amorphous structure. As shown in Fig. 3, the corrosion-resistant layer d2 on the insulating window 204 has a high thickness, a compact texture, a smooth surface, and no holes are formed. A plasma enhanced physical vapor deposition (PEPVD) process is capable of producing a corrosion resistant coating d2 having a good or compact grain structure and a random crystal orientation.

Typically, the rate of heating should be less than 3 ° C per minute. Typically, the heating temperature should range from 100 ° C to 750 ° C or even higher, and the heating time should range from 10 min to 12 h or more. The timing and conditions of the above thermal annealing step should depend on the thickness of the desired corrosion resistant coating, the thickness and size of the insulating window, and the like.

Further, the material of the anti-corrosion layer coating layer includes any one or more of the following: Y ₂ O ₃ , YF ₃ , ErO ₂ , Al ₂ O ₃ , SiC, AlN, ZrO ₂ . Further, the ceramic substrate of the insulating window 204 is quartz or aluminum oxide. Further, the anti-corrosion coating has a thickness of more than 40 um, such as 45 um, 50 um, 58 um, 63.5 um, 100 um, and the like.

According to a variant of the invention, the corrosion-resistant layer coating has a multilayer structure. The anti-corrosion coating has a multi-layer structure in which a residual stress of the anti-corrosion layer is released in an interface between the multilayer structures, and thus a thick and dense anti-corrosion layer can be Adhered to the insulating window 204 with good adhesion and performance. When the corrosion-resistant coating has a multilayer structure, the thickness of each of the single-layer structures in the multilayer structure ranges from 0.1 um to 30 um, and the number of the multilayer structures can reach from 1 to 100 layers. In accordance with a preferred embodiment of the present invention, each of the most preferred single layer materials is compounded to form a multi-layered corrosion resistant coating having a thickness that can be increased to 60 um and above using enhanced physical or chemical vapor deposition. The increase in the interface between the multilayer structures can effectively reduce the residual stress of the coating caused by the multilayer material structure (e.g., different crystal structures or elastic modulus) or different material properties (e.g., different coefficients of thermal expansion). A plurality of anti-corrosion coatings are deposited on the insulating window 204 such that the insulating window 204 coated with the anti-corrosion coating has an increased coating thickness, a stable surface facing plasma chemistry, and an intended function to improve plasma processing. Process performance of the chamber. Different from the structure of a single-layer coating, the same material is deposited but the coating structure with a multi-layer structure can achieve an increased thickness, and the coating stress can be released due to the increased interface area of the multilayer structure (the coating stress usually follows the material) The thickness of the layer or coating increases and the risk of cracking or cracking is reduced. Among them, the top layer material of the multilayer material structure is inevitably an anti-corrosion coating material to overcome the corrosion of the plasma process environment.

As shown in FIG. 4, a second aspect of the present invention provides a method of manufacturing an insulating window 204 of a corrosion-resistant inductively coupled plasma processing chamber 200, wherein the manufacturing method includes the following steps: first, step S11 is performed. Providing an insulating window 204 substrate; then performing step S12, applying a layer of anti-corrosion coating d2 on the plasma-facing side 204a of the insulating window 204 substrate by using enhanced physical or chemical vapor deposition; The insulating window 204 covered with the anti-corrosion coating d2 performs a heat treatment step. According to a specific embodiment of the present invention, the heat treatment step includes a thermal annealing treatment.

Figure 5 is a schematic diagram of the principle of a PEPVD for a method of fabricating an insulating window of an anti-corrosion inductively coupled plasma processing chamber in accordance with an embodiment of the present invention. Specifically, wherein the enhanced physical or chemical vapor deposition is performed in a low pressure or vacuum chamber environment, wherein at least one of the deposited elements or components is evaporated or sputtered from a source of material, evaporated or sputtered out The material is concentrated on the surface of the insulating window 204. This part of the process is a physical process, referred to herein as physical vapor deposition or PVD. At the same time, one or more plasma sources are used to emit ions or generate a plasma to surround the surface of the gas showerhead, at least one of the deposited elements or components being ionized and with the element or component being vaporized or sputtered in the plasma or The reaction is carried out on the surface of the gas shower head. Thus, the insulating window 204 is coupled to a negative voltage such that it is bombarded by ionized atoms or ions during the deposition process, which is a "plasma enhanced" (PE) function in PEPVD.

A source material 820 includes components to be deposited, which are typically in solid form. For example, if the film to be deposited is Y2O3 or YF3, the source material 820 should include germanium (or fluorine) - possibly other materials such as oxygen, fluorine (or helium), and the like. To form a physical deposit, the source material is evaporated or sputtered. In the particular embodiment illustrated in FIG. 1, evaporation is performed using an electron gun 825 that directs an electron beam 830 over the source material 820. When the source material is evaporated, the atomic and molecular locations drift toward the component insulating window 204 to be coated and condense on the component insulating window 204 to be coated, shown by the dashed arrows in the illustration.

The plasma enhanced component is comprised of a gas injector 212 that injects an active or inactive source gas, such as a gas comprising argon, oxygen, fluorine, into the chamber 100, shown in phantom in the drawing. The plasma is maintained in front of the insulating window 204 using a plasma source, such as a radio frequency, microwave, etc., in this embodiment exemplarily coupled to a radio frequency The coil 121 of the source 214 is shown. Without being bound by theory, we believe that several processes occur in the PE section. First, an inactive ionized gas component, such as argon, bombards the insulating window 204 as it is gathered to cause the film to become dense. The effect of ion bombardment results from the application of a negative bias to the insulating window 204, or from ions emitted by the plasma source and aligned with the insulating window 204. Furthermore, reactive gas components or radicals, such as oxygen or fluorine, react with the evaporated or sputtered source material, either on the surface of the insulating window 204 or in the chamber. For example, the source material ruthenium reacts with oxygen to form a ruthenium-containing coating such as Y2O3 or YF3. Thus, the above processes have physical processes (bombardment and condensation) and chemical processes (eg, oxidation and ionization).

Wherein, the above plasma source can be used to ionize, decompose and excite the reaction gas to enable the deposition process to be performed at a low substrate temperature and a high coating growth rate (due to the plasma generating more ions and radicals), Or it is used to generate energetic ions for the insulating window 204 such that the ions bombard the surface of the insulating window 204 and help form a thick and concentrated anti-corrosion coating thereon.

Further, the manufacturing method further includes performing the following steps between steps S12 and S13: performing a roughening treatment step on one side of the insulating window 204 exposed to the plasma, and then utilizing enhanced physical or chemical on the insulating window 204 substrate. The vapor deposition is coated with a corrosion resistant coating on its plasma facing side 204a.

One possible condition is that the corrosion resistant coating applied to the insulating window has compressive stress and the insulating window 204 has a higher stress. Typically, the thermal annealing step includes a heat treatment. By maintaining the insulating window 204 coated with the anti-corrosion coating at a specific temperature and heat for a period of time, the stress can be effectively reduced. This is due to microstructural defects in the corrosion resistant coating, such as displacing, grain boundaries, and uneven distribution of atoms in the crystal or interface regions. Above resistance Microstructural defects in the corrosion coating can be reduced or eliminated by atomic diffusion. Therefore, the thermal annealing step can explain the reduction of the residual stress of the corrosion-resistant coating, thereby improving the structural stability of the corrosion-resistant coating.

Optionally, the surface roughness of the insulating window 204 is less than 0.5 um, so that a corrosion-resistant coating is applied on the surface thereof, for example, roughness of 0.45 um, 0.3 um, 0.32 um, 0.28 um, 0.25 um, 0.13 um, etc. .

Optionally, the surface roughness of the insulating window is greater than 2 um, such as 2.8, 3, 3.53, 4.85, 5.83, and the like. When the corrosion-resistant coating is dense and the thickness reaches 40 um or more, the insulating window with a relatively large roughness can have good adhesion against the corrosion coating. This is due to the increase in the surface roughness of the insulating window, which increases the contact area of the interface between the anti-corrosion coating and the surface of the substrate, and changes the contact area of the anti-corrosion coating from a 2-dimensional fraction to a three-dimensional fragment ( 3-dimensional fraction). The deposition of a corrosion-resistant coating on the rough surface can result in the formation of a random crystal orientation of the coating and lead to the release of interface stress between the corrosion-resistant coating and the insulating window 204 substrate, which enhances the insulating window 204 substrate and the corrosion-resistant coating. The adsorption force promotes the formation of a thick and dense coating thereon.

Further, when the anti-corrosion coating has a multi-layered structure, the manufacturing method further includes the step of: performing a thermal annealing treatment step on the insulating window 204 coated with the anti-corrosion coating, on the insulating window The multi-layered anti-corrosion coating is surface-polished or ground. In combination with surface roughness trimming and multilayer structure formation, a plasma anti-corrosion coating having a higher thickness can be deposited on the insulating window with enhanced interface adhesion. Reducing the roughness of the surface can help reduce polymer deposition during the process and therefore reduce metal contamination. Typically, the surface of the insulating window can be ground or polished The process needs to have a specific roughness, preferably below 0.1 um. Alternatively, roughening treatment is carried out by slurry cleaning, aerosol cleaning, blasting against corrosion coating or insulating window surfaces. The roughened surface treatment described above can repair the deposition of the insulating window surface to reduce particle contamination in the etching process. The surface treatment steps such as the above polishing or grinding or roughening treatment may be performed before or after the thermal annealing step according to the process requirements.

Further, the temperature at which the corrosion-resistant coating is made by enhanced physical or chemical vapor deposition ranges from room temperature to 300 ° C or higher. Among them, the process coefficients of enhanced physical or chemical vapor deposition include temperature, pressure, and power are adjustable, which are adjusted to form a good adhesion anti-corrosion coating, and optionally form a corrosion-resistant coating to be smooth. Or a rough surface, optionally forming a corrosion resistant layer as a single or multi-layer structure.

Further, the present invention can also perform a reprocessing step on the insulating window 204 coated with the anti-corrosion coating to increase its service life and cost. One of the reprocessing steps is to machine the surface of the insulating window 204. The reprocessing step is performed on the used insulating window, wherein the surface of the insulating window 204 is damaged by the plasma, or the coating on the surface thereof is overlapped or contaminated by the deposit in the plasma etching process, thus performing The reprocessed insulating window 204 can be used for a longer period of time, and its production cost is reduced.

Further, the anti-corrosion coating has different surface characteristics, such as setting a specific surface roughness such that a thick and dense anti-corrosion coating can adhere to the insulating window with good adhesion. The service life of the insulating window coated with the anti-corrosion coating obtained by multi-layer coating or polishing described above is also correspondingly extended.

The thermal annealing step and its technical effects will be described in detail below. See section 6 Figure 6 is a schematic diagram showing the principle of a thermal annealing step of a method for manufacturing an insulating window of an anti-corrosion inductively coupled plasma processing chamber according to an embodiment of the present invention, wherein the abscissa represents time and the ordinate represents temperature. As shown in the figure, the insulating window 204 of the inductively coupled plasma processing chamber made of yttrium oxide is an example of a processing element. First, the insulating window 204 is sent to a thermal annealing furnace at 2 ° C or min for a period of t1. The speed of the insulating window 204 is raised to 400 ° C, then the insulating window 204 is maintained at 400 ° C for the next 3 hours, and finally the temperature of the insulating window 204 is measured at a rate of 1 ° C or min during the t2 period. Reduce to 0. It should be noted that the t1 and t2 time periods are only schematically represented for a period of time herein, and the specific materials of t1 and t2 are not specifically limited, as long as the temperature at which the temperature of the insulating window 204 is raised or lowered is controlled within a certain range, And finally reach the maximum temperature or reduce to 0.

Those skilled in the art will appreciate that the specific parameter requirements, including time, maximum temperature, rate of temperature rise, rate of temperature drop, etc., performed by the thermal annealing step are determined by the particular material and its number of layers. Figure 7 is a list of parameters for a thermal annealing step of a method of fabricating an insulating window of a corrosion-resistant inductively coupled plasma processing chamber for different material layers in accordance with an embodiment of the present invention. As shown in the table illustrated in Fig. 7, when the material is selected to be anodized Al, and the final thickness is required to be 75 um, and the number of layers is one, the thermal annealing step needs to be maintained at 200 ° C for 4 h. The initial stress was 3.27 GPa before the thermal annealing step, and the subsequent stress after the thermal annealing step was 2.71, and the stress reduction was 17%. When the material is selected to be Al ₂ O ₃ and the final thickness is required to be 75 μm and the number of layers is 4, the thermal annealing step needs to be maintained at 400 ° C for 3 h. The initial stress was 3.13 GPa before the thermal annealing step was performed, and the subsequent stress after the thermal annealing step was 2.24, and the stress reduction was 28%. When the material is selected to be Al and the final thickness is required to be 90 um and the number of layers is 2, the thermal annealing step needs to be maintained at 200 ° C for 4 h. The initial stress was 1.97 GPa before the thermal annealing step, and the subsequent stress after the thermal annealing step was 1.71, and the stress reduction was 13%. When the material is selected to be Al and the final thickness is required to be 130 um and the number of layers is 4, the thermal annealing step needs to be maintained at 200 ° C for 4 h. The initial stress was 3.82 GPa before the thermal annealing step, and the subsequent stress after the thermal annealing step was 2.53, and the stress reduction was 34%. Thus, it can be seen that the thermal annealing step provided by the method of the present invention has a significant effect on stress reduction of various materials, which illustrates the superiority of the present invention.

We also analyzed the stress changes through the Bragg principle. Figure 8 is a schematic diagram of the principle of Bragg. As shown in Figure 8, the anti-corrosion layer d2 on the insulating window 204 of the inductively coupled plasma processing chamber which is produced by the method for manufacturing an insulating window provided by the present invention utilizes the principle of Bragg Performing an analysis, specifically, at least two X-ray rays S11 and S21 are incident from the upper surface of the anti-corrosion layer d2 to the upper surface and the lower surface of the anti-corrosion layer d2, and after being reflected and diffracted, respectively, the reflected light S12 and the diffracted light S22 are obtained. . Therefore, the X-ray rays on the upper surface are reflected, and the X-ray rays on the lower surface are diffracted. Where θ is the diffraction angle (Brag angle), λ is the X-ray wavelength, 2d is the crystal plane distance, and S=d*sinθ. According to the Bragg principle, if there is no stress, the 2θ angle and the crystal plane distance d of the same (hkl) crystal plane do not change under different dip angles (PSI). If there is residual stress, the 2θ angle and the crystal plane distance d of the same (hkl) crystal plane change with the inclination angle 在 under different tilt angles (PSI). If it is tensile stress, the larger the Ψ, the larger d. In the case of compressive stress, the larger the enthalpy, the smaller d is. If it is an ideal plane stress state, the following relationship is obtained: σ = K ̇ M

Where E is the Young's modulus and E = 171.5 GPa. v is Poisson's ratio, v = 0.298. M is the change of the 2θ value of the same crystal plane under a plurality of transfer ψ conditions, and the slope is obtained by straight line fitting, and the slope is M of the above relational expression.

Fig. 9 is a graph showing the slope M obtained by straight line fitting using the principle of Bragg. The abscissa indicates Sin ² ψ and the ordinate is 2θ. As shown, the slope M = 0.5614 is obtained. Therefore, it can be known that under different tilt angles (PSI), the 2θ angle of the same (hkl) crystal plane and the crystal plane distance d change little, so that the present invention has a remarkable effect on stress reduction.

Although the present invention has been described in detail by the preferred embodiments thereof, it should be understood that the foregoing description should not be construed as limiting. Various modifications and alterations of the present invention will be apparent to those skilled in the art. Therefore, the scope of the invention should be defined by the appended claims. In addition, any reference signs in the claims should not be construed as limiting the claims; the word "comprising" does not exclude the means or steps that are not listed in the other claims or the description; "first", " Words such as "two" are used only to denote a name, and do not denote any particular order.

Claims (14)

An insulating window of an anti-corrosion inductively coupled plasma processing chamber, characterized in that: the insulating window is coated with a corrosion-resistant coating on a side facing the plasma by plasma enhanced physical vapor deposition. The insulating window coated with the anti-corrosion coating is subjected to a heat treatment step; the anti-corrosion layer coating has a multilayer structure, and the anti-corrosion coating has a thickness of more than 40 um. The insulating window of claim 1, wherein the heat treatment step comprises a thermal annealing treatment. The insulating window according to claim 2, wherein: the material of the anti-corrosion layer coating comprises any one or more of the following: Y ₂ O ₃ , YF ₃ , ErO ₂ , Al ₂ O ₃ , SiC, AlN, ZrO ₂ . The insulating window according to claim 3, wherein the anti-corrosion layer coating has a multi-layer structure. The insulating window according to claim 2, wherein the ceramic substrate of the insulating window is quartz or alumina. A method of manufacturing an insulating window of an inductively coupled plasma processing chamber, wherein the manufacturing method comprises the steps of: providing an insulating window substrate in a low pressure or vacuum chamber environment; Applying a layer of anti-corrosion coating on the substrate facing the plasma by using enhanced physical or chemical vapor deposition on the substrate; the enhanced physical vapor deposition method is: placing a material source in the low pressure or vacuum chamber In the chamber environment, the source of material is evaporated or sputtered such that the evaporated or sputtered material concentrates on the surface of the substrate of the insulating window; at the same time, an active and inactive plasma is injected into the low pressure or vacuum chamber environment. a source, the reactive plasma reacting with the evaporated or sputtered source material, the inactive plasma bombarding the surface of the insulating window such that the evaporated or sputtered material concentrates on the surface of the insulating window substrate becomes dense; A heat treatment step is performed on the insulating window coated with the anti-corrosion coating. The manufacturing method of claim 6, wherein the heat treatment step comprises a thermal annealing treatment. The manufacturing method according to claim 7, wherein the manufacturing method further comprises the steps of: roughening a side of the insulating window exposed to the plasma, and then utilizing the enhanced type on the insulating window substrate; Physical vapor deposition is coated with a corrosion resistant coating on one side of the plasma. The manufacturing method of claim 8, wherein the roughening treatment causes the surface roughness of the insulating window to be less than 0.5 um. The manufacturing method of claim 8, wherein the roughening treatment causes the surface roughness of the insulating window to be greater than 2 um. The manufacturing method according to claim 7, wherein when the anti-corrosion coating has a multi-layered structure, the manufacturing method further comprises the step of performing heat on the insulating window coated with the anti-corrosion coating. After the annealing step, the multi-layered anti-corrosion coating on the insulating window is surface-polished or ground. The manufacturing method according to claim 7, wherein the temperature of the anticorrosive coating layer formed by the enhanced physical vapor deposition is in a range of higher than room temperature. The manufacturing method of claim 7, wherein the corrosion-resistant coating has a thickness of more than 40 um. The manufacturing method according to claim 7, wherein when the corrosion-resistant coating has a multi-layered structure, the thickness of each of the single-layer structures in the multilayer structure ranges from 0.1 um to 30 um, and the multilayer structure The number can reach 1 to 100 layers.