CN105088141A - Inductive coupling type plasma processing chamber, anti-corrosion insulation window of inductive coupling type plasma processing chamber and manufacturing method of anti-corrosion insulation window - Google Patents
Inductive coupling type plasma processing chamber, anti-corrosion insulation window of inductive coupling type plasma processing chamber and manufacturing method of anti-corrosion insulation window Download PDFInfo
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- CN105088141A CN105088141A CN201410222472.1A CN201410222472A CN105088141A CN 105088141 A CN105088141 A CN 105088141A CN 201410222472 A CN201410222472 A CN 201410222472A CN 105088141 A CN105088141 A CN 105088141A
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Abstract
The invention provides an inductive coupling type plasma processing chamber, an anti-corrosion insulation window of the inductive coupling type plasma processing chamber and a manufacturing method of the anti-corrosion insulation window. The face, facing plasma, of the insulation window is coated with an anti-corrosion coating through enhanced physical or chemical vapor deposition, and heat treatment is carried out on the insulation window coated with the anti-corrosion coating. Heat treatment comprises the step of heat annealing. The manufactured anti-corrosion coating is large in thickness, even in texture, stable in structure and low in stress and cannot be broken.
Description
Technical field
The present invention relates to field of semiconductor manufacture, particularly relate to a kind of jigger coupling type plasma process chamber and anticorrosive insulated window thereof and manufacture method.
Background technology
Plasma process chamber utilizes the principle of work of vacuum reaction chamber to carry out the processing of the substrate of semiconductor chip and plasma flat-plate.The principle of work of vacuum reaction chamber is in vacuum reaction chamber, pass into the reactant gases containing suitable etchant source gas, and then radio-frequency (RF) energy input is carried out to this vacuum reaction chamber, with activated reactive gas, excite and maintain plasma, so that the material layer etched respectively on substrate surface or over the substrate surface depositing layer of material, and then semiconductor chip and plasma flat-plate are processed.
Owing to there is plasma body in plasma process chamber, plasma process chamber is exposed to the corrosion that the assembly of plasma body or chamber wall all can be subject in various degree.It is also proposed in the industry the mechanism of different manufacture corrosion resistant components.
How manufacturing reliable and stable corrosion resistant component, is the target that those skilled in the art research and develop.
Summary of the invention
For the problems referred to above in background technology, the present invention proposes a kind of jigger coupling type plasma process chamber and anticorrosive insulated window thereof and manufacture method.
First aspect present invention provides a kind of insulated window of erosion-resisting jigger coupling type plasma process chamber, wherein: described insulated window utilizes enhancement type physics or chemical vapour deposition at its coating of one side in the face of plasma body corrosion-resistant coating, the insulated window being coated with corrosion-resistant coating described in has carried out heat treatment step.
Further, described heat treatment step comprises thermal anneal process.
Further, the material of described etch resistant layer coating comprise following any one or appoint multiple: Y
2o
3, YF
3, ErO
2, Al
2o
3, SiC, AlN, ZrO
2.
Further, the thickness of described corrosion-resistant coating is for being greater than 40um.
Further, described etch resistant layer coating has multilayered structure.
Further, the ceramic matrix of described insulated window is quartz or aluminum oxide.
Second aspect present invention provides a kind of manufacture method of insulated window of erosion-resisting jigger coupling type plasma process chamber, and wherein, described manufacture method comprises the steps:
One insulated window matrix is provided;
Described insulated window matrix utilize enhancement type physics or chemical vapour deposition are coated with one deck corrosion-resistant coating in its one side in the face of plasma body;
Then heat treatment step is performed to the insulated window being coated with corrosion-resistant coating.
Further, described heat treatment step comprises thermal anneal process.
Further, described manufacture method also comprises the steps: that one side insulated window being exposed to plasma body carries out roughened step, on described insulated window matrix, then utilize enhancement type physics or chemical vapour deposition to be coated with one deck corrosion-resistant coating in its one side in the face of plasma body.
Further, described roughened makes the surfaceness of insulated window be less than 0.5um.
Further, described roughened makes the surfaceness of insulated window be greater than 2um.
Further, when described corrosion-resistant coating has multilayered structure, described manufacture method also comprises the steps:, after performing thermal anneal processing step to the insulated window being coated with corrosion-resistant coating, to carry out surface finish or milled processed to the corrosion-resistant coating of the multilayered structure on insulated window.
Further, the temperature span utilizing enhancement type physics or chemical vapour deposition to manufacture corrosion-resistant coating is higher than room temperature.
Further, the thickness of described corrosion-resistant coating is for being greater than 40um.
Further, when described corrosion-resistant coating has multilayered structure, the Thickness scope of the every one deck single layer structure in its multilayered structure is 0.1um to 30um, and the number of multilayered structure can reach 1 to 100 layers.
According to the present invention's specific embodiment, the present invention adopts the corrosion-resistant coating of enhancement type physics or chemical vapour deposition deposition to have higher caliper, and insulated window performs thermal anneal step, with the stable structural stability being coated with the insulated window of coating.Due to differing materials and utilize enhancement type physics or chemical vapour deposition to form corrosion-resistant coating under ion bombardment effects, the corrosion-resistant coating that insulated window applies must have residual stress.
Accompanying drawing explanation
Fig. 1 is the structural representation of jigger coupling type plasma process chamber;
Fig. 2 a is the diagrammatic cross-section of the method manufacture top coat of the using plasma spraying of the insulated window of the jigger coupling type plasma process chamber of prior art;
Fig. 2 b is that the method for the direct doped yttrium oxide of block ceramic that utilizes of the insulated window of the jigger coupling type plasma process chamber of prior art manufactures the diagrammatic cross-section of top coat;
Fig. 3 is the cross-sectional view of the insulated window of erosion-resisting jigger coupling type plasma process chamber according to the present invention's specific embodiment;
Fig. 4 is the manufacture method flow chart of steps of the insulated window of a kind of erosion-resisting jigger coupling type plasma process chamber according to the present invention's specific embodiment;
Fig. 5 is the principle schematic of the PEPVD of the manufacture method of the insulated window of a kind of erosion-resisting jigger coupling type plasma process chamber according to the present invention's specific embodiment;
Fig. 6 is the curve principle schematic of the thermal anneal step of the manufacture method of the insulated window of a kind of erosion-resisting jigger coupling type plasma process chamber according to the present invention's specific embodiment;
Fig. 7 is the parameter list of thermal anneal step for different material layer of the manufacture method of the insulated window of a kind of erosion-resisting jigger coupling type plasma process chamber according to the present invention's specific embodiment;
Fig. 8 is Prague principle schematic;
Fig. 9 is the graphic representation utilizing Prague principle to carry out fitting of a straight line to ask slope to analyze invention effect of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described.
It is to be noted; " semiconductor arts piece ", " wafer " and " substrate " these words often will be exchanged use in explanation subsequently; in the present invention; they all refer to that, in the processed process conditions of process chamber, process conditions is not limited to wafer, substrate, substrate, large-area flat-plate substrate etc.For convenience of description, mainly exemplary illustration will be made for " substrate " herein in embodiment illustrates and illustrates.
The present invention to be applicable in all plasma process chamber, easily by the assembly of plasma etching, comprise capacitive coupling plasma treatment chamber (CCP) and capacitive coupling plasma treatment chamber (ICP).Such as, the gas spray (showerhead) of capacitive coupling plasma treatment chamber, and the position such as various chamber sidewall top boards.Hereafter be described for the insulated window of condenser coupling plasma process chamber.It should be noted that, although be described for the insulated window of condenser coupling plasma process chamber herein, it can not be used for limiting the present invention, and range of application of the present invention is not limited thereto.
Fig. 1 is the structural representation of the inductance coupling plasma processing device according to the present invention's specific embodiment.Fig. 2 illustrates plasma treatment appts 200 according to an embodiment of the invention.Should be appreciated that inductance coupling plasma processing device 200 is wherein only exemplary, described 200 in fact also can comprise less or extra parts, and the arrangement of parts also can be different from shown in Fig. 2.
Fig. 1 shows the sectional view of inductance coupling plasma processing device according to a first embodiment of the present invention.Inductance coupling plasma processing device 200 comprises metal sidewall 202 and insulation top board 204, forms an airtight vacuum sealing housing, and is vacuumized by vacuum pumping pump (not shown).Described insulation top board 204 only exemplarily, also can adopt other top board pattern, and such as dome shape, with the metal top plate etc. of insulating material window.Pedestal 206 comprises an electrostatic chuck (not shown), described electrostatic chuck is placed pending substrate W.Bias power is applied on described electrostatic chuck, to produce the holding force to substrate W.The radio frequency power of radio-frequency power supply 208 be applied to be positioned at insulation top board 204 on radio frequency power launching device on.Wherein, in the present embodiment, described RF transmitter comprises radio-frequency coil 210.Process gas is supplied in reaction chamber from source of the gas through pipeline, to light and to maintain plasma, thus processes substrate W.Preferably, process gas and enter chamber from gas inject mouth 212.
See Fig. 1, known, the back side of insulated window 204 is directly exposed to process zone P, under the corrosion being in the plasma body in process zone P for a long time.Therefore, prior art also uses a lot of Corrosion resistance mechanism and attempts to address this problem, but also brings new problem.Such as, aluminium oxide Al is utilized
2o
3the insulated window 204 manufactured can cause Al metallic pollution, metallic pollution is avoiding greatly in plasma process chamber, insulated window 204 is positioned at directly over substrate W, if metallic pollution drops on substrate W from insulated window 204, will cause irreversible damage to substrate.And with quartz manufacture insulated window often work-ing life short.
In order to produce reliable and stable insulated window, slip-stick artist have employed many different methods to manufacture the jigger coupling type plasma body insulated window with an etch resistant layer.Fig. 2 a is the diagrammatic cross-section of the method manufacture top coat of the using plasma spraying of the insulated window of the jigger coupling type plasma process chamber of prior art.As shown in Figure 2 a, the corrosion-resistant coating d11 utilizing plasma spraying (plasmaspray) manufacture to be coated on the surperficial 104a of insulated window 104 is formed owing to utilizing the yttrium oxide particle of spraying, quality is soft, and there is vesicular open texture, wherein there is a lot of hole a as shown in Figure 2.The corrosion-resistant coating d11 utilizing plasma spraying (plasmaspray) to manufacture causes the coating formed to have high surfaceness (Ra be greater than 4 microns or more) and correspondingly highly porous (volume fraction is greater than 3%) usually, easily produces particle contamination in plasma environment.In addition, owing to also comprising other gases in hole a, such as nitrogen etc., the corrosion resistant material purity of etch resistant layer d11 is declined very many, as etch resistant layer d11 because corrosive nature is thinning gradually, the gas in hole a can be released gradually, also can become the foreign gas in substrate processing procedure process.Therefore, prior art utilizes the insulated window etch resistant layer d11 of plasma spray process manufacture to have high roughness and vesicular structure, and make insulated window 104 or etch resistant layer easily produce particle, it likely causes the pollution of processing procedure substrate.In addition; due to the plasma spray coating in gas injection hole very coarse and and the matrix of insulated window 104 there is more weak adhesive power; when this used in plasma treatment chamber by spray coated gas spray time, described particle can from gas inject mouth out, drop on substrate.
Fig. 2 b is the diagrammatic cross-section of the method manufacture top coat of the direct doped yttrium oxide of employing block ceramic of the insulated window of the jigger coupling type plasma process chamber of prior art, it utilizes the direct doped yttrium oxide corrosion resistant material of block ceramic to manufacture insulated window 104, but insulated window 104 thermal shock resistance manufactured like this is poor, there is larger Cracking Failure risk.As shown in Figure 2 b, still there is a lot of hole a in the insulated window 104 manufactured like this.
In addition, slip-stick artist also adopts many additive methods to manufacture insulated window, such as block yttria-base pottery sosoloid or complex phase ceramic, but manufacturing cost is very high.Again such as, the insulated window of composite structural ceramic, as with aluminum oxide and yttrium oxide double-deck powder sintering press ceramic window, processed complex, cost is high.
In order to solve the defect occurred above, the insulated window 204 of a kind of erosion-resisting jigger coupling type plasma process chamber 200 of the present invention, to improve by the performance of the jigger coupling type plasma process chamber 200 of aluminum oxide processing procedure.Fig. 3 is the insulated window of jigger coupling type plasma process chamber according to the present invention's specific embodiment and the diagrammatic cross-section of corrosion-resistant coating thereof, the present invention utilizes the one side 204a of plasma-enhanced physics or chemical vapour deposition (PEPVD or PECVD) processing procedure plasma on insulated window 204 to deposited thick layer and the corrosion-resistant coating d2 of densification, has then carried out heat treatment step to the described insulated window 204 being coated with corrosion-resistant coating.
According to a preferred embodiment of the present invention, described heat treatment step comprises thermal anneal process.Although the corrosion-resistant coating of enhancement type physics or chemical vapour deposition deposition can reach higher caliper, but the structure stability in corrosion-resistant coating is not good enough, crystal combination degree defectiveness between atom, there is higher stress, such corrosion-resistant coating easily ftractures, the etch resistant layer of cracking is easily dropped become particle contamination or metallic pollution by processing procedure plasma bombardment in chamber in processing procedure process, even drops on substrate W, substrate W to be scrapped.Thermal anneal step can make mutually to shake between the atom in corrosion-resistant coating, fills up void, makes to combine tightr each other.The etch resistant layer thickness that the present invention utilizes enhancement type physics or chemical vapour deposition to manufacture is thick, and tight in structure, it has good fine and close atomic structure or undefined structure.As shown in Figure 3, the etch resistant layer d2 thickness on insulated window 204 is high, and quality is tight, and smooth surface, does not produce any hole.Plasma-enhanced physical vapor deposition (PEPVD) technique can manufacture one and have good or tight particle structure and random crystal orientation (randomcrystalorientation) corrosion-resistant coating d2.
Typically, the speed of heating should be less than 3 DEG C or min.Typically, the span of Heating temperature should be even higher to 750 DEG C at 100 DEG C, and the span of heat-up time should at 10min to 12h or more of a specified duration.The time of above-mentioned thermal anneal step and condition should depend on the thickness of required corrosion-resistant coating, the thickness of insulated window and size etc.
Further, the material of described etch resistant layer coating comprise following any one or appoint multiple: Y
2o
3, YF
3, ErO
2, Al
2o
3, SiC, AlN, ZrO
2.Further, the ceramic matrix of described insulated window 204 is quartz or aluminum oxide.Further, the thickness of described corrosion-resistant coating for being greater than 40um, such as 45um, 50um, 58um, 63.5um, 100um etc.
According to the present invention's variation, described etch resistant layer coating has multilayered structure.Described corrosion-resistant coating has multilayered structure, wherein, the residual stress (residualstress) of described etch resistant layer in multilayered structure between interface obtain release, the therefore thick and etch resistant layer of densification can adhere on insulated window 204 with good adhesive power and performance.When described corrosion-resistant coating has multilayered structure, the Thickness scope of the every one deck single layer structure in its multilayered structure is 0.1um to 30um, and the number of multilayered structure can reach 1 to 100 layers.In accordance with a preferred embodiment of the present invention, being combined with each other by most preferred each monolayer material to be formed has the corrosion-resistant coating of certain thickness multilayered structure, its thickness can utilize enhancement type physics or chemical vapour deposition reach 60um and more than.Between multilayered structure, the increase at interface can reduce the coating residual stress brought by multi-layered material structure (such as different crystal structure or Young's modulus) or dissimilar material properties (such as different thermal expansivity) effectively.Insulated window 204 deposits multilayer corrosion-resistant coating, with make the insulated window 204 of coated corrosion-resistant coating have increase coat-thickness, in the face of the surface of stability of plasma chemistry and expectation function, to improve the processing procedure performance of plasma process chamber.Be different from the structure of single-layer coating, same material is deposited but the coating structure with multilayered structure can reach the thickness of increase, the interfacial area increased due to multilayered structure can release coat stress (described coating stress increases along with the thickness of material layer or coating increases usually), and it produces crack or the risk of splitting is lowered.Wherein, the quilting material necessarily corrosion-resistant coating material of multi-layered material structure, to overcome the corrosion of plasma processing environment.
As shown in Figure 4, second aspect present invention provides a kind of manufacture method of insulated window 204 of erosion-resisting jigger coupling type plasma process chamber 200, wherein, described manufacture method comprises the steps: first to perform step S11, provides insulated window 204 matrix; Then perform step S12, described insulated window 204 matrix utilizes enhancing physics or chemical vapour deposition on the one side 204a of plasma body, are coated with one deck corrosion-resistant coating d2 at it; Then perform heat treatment step according to the present invention's specific embodiment to the insulated window 204 being coated with corrosion-resistant coating d2, described heat treatment step comprises thermal anneal process.
Fig. 5 is the principle schematic of the PEPVD of the manufacture method of the insulated window of a kind of erosion-resisting jigger coupling type plasma process chamber according to the present invention's specific embodiment.Particularly, wherein, described enhancement type physics or chemical vapour deposition perform under low pressure or vacuum chamber environment, wherein at least one deposition of elements or composition are evaporated from a material source or are sputtered out, the material evaporated or sputter out is concentrated in the matrix surface of insulated window 204, this part processing procedure is a physical process, is called as physical vapor deposition or PVD part here.Simultaneously, one or more plasma source is used to send ion or produces plasma body with around gas shower head surface, and at least one deposition of elements or composition are ionized and react on the surface in the plasma or at gas spray with the element evaporated or sputter or composition.Thus insulated window 204 is coupled to negative voltage, make it in deposition manufacture process process, be ionized atom or ion bombardment, this is " plasma enhancing " (plasmaenhanced, or the PE) function in PEPVD.
One source material 820 comprises component to be deposited, it typically is solid form.Such as, if film to be deposited is Y2O3 or YF3, source material 820 should comprise yttrium (or fluorine)---other material may be also had, such as oxygen, fluorine (or yttrium) etc.In order to form physical deposition, described source material is evaporated or is sputtered.In the specific embodiment shown in Fig. 1, utilize electron beam gun (electrongun) 825 to perform evaporation, it is by electron beam (electronbeam) 830 pilot source material 820.When source material is evaporated, atom and molecular position are to part insulates window 204 to be coated drift and be condensed on part insulates window 204 to be coated, illustrate in diagram with dotted arrow.
Plasma-enhanced parts are made up of gas inject mouth (gasinjector) 212, and it injects active or nonactive source gas in chamber 100, such as, comprise the gas of argon, oxygen, fluorine, be shown in broken lines in diagram.Plasma body utilizes plasma source to be maintained at the front of insulated window 204, and plasma source is radio frequency, microwave etc. such as, is exemplarily illustrated by the coil 121 being coupled in radio frequency source 214 in the present embodiment.Not bound by theory, we think PE part have several process to occur.First, non-reactive ions oxidizing gases component, such as argon, bombardment insulated window 204, when it is aggregated after thus make film become densification.The effect of ion bombardment stems from negative bias and is applied to insulated window 204, or stem from sent by plasma source and aim at the ion of insulated window 204.In addition, the reactive gas component of such as oxygen or fluorine or free radical and evaporation or the source material that sputters react, described reaction or be positioned at insulated window 204 surface on or be positioned at chamber.Such as, source material yttrium and oxygen reaction generate yttrium-containing coatings, such as Y2O3 or YF3.Therefore, above-mentioned processing procedure has physical process (bombardment and condensation) and chemical process (such as, oxidation and ionizing).
Wherein, above-mentioned plasma source can be used to ionization, decomposition and provocative reaction gas can perform (due to the more ion of plasma generation and free radical) to make deposition manufacture process under low underlayer temperature and the high coating speed of growth, or be used to produce for the energetic ion (energeticions) of insulated window 204, with make the surface of ion bombardment insulated window 204 and contribute on form thick and concentrated corrosion-resistant coating.
Further, described manufacture method is also included between step S12 and S13 and performs following steps: one side insulated window 204 being exposed to plasma body carries out roughened step, on described insulated window 204 matrix, then utilize the one side 204a strengthening physics or chemical vapour deposition plasma body faced by it to apply one deck corrosion-resistant coating.
Wherein a kind of possible situation is that the corrosion-resistant coating be coated on insulated window has compression stress and insulated window 204 has higher stress.Typically, thermal anneal step comprises thermal treatment.By being coated with the insulated window 204 of corrosion-resistant coating under for some time remains on specified temp and temperature, then effectively can reduce stress.This is due to the microstructural defects in corrosion-resistant coating, the displacement of such as atom in crystal or interface zone, crystal boundary and uneven distribution.Microstructural defects in above-mentioned corrosion-resistant coating can be reduced by atomic diffusion and even eliminate.Therefore, thermal anneal step can help the residual stress reducing corrosion-resistant coating, therefore, it is possible to improve the structural stability of corrosion-resistant coating.
Alternatively, the surfaceness of insulated window 204 is less than 0.5um, after making, apply corrosion-resistant coating in its surface, and such as roughness is 0.45um, 0.3um, 0.32um, 0.28um, 0.25um, 0.13um etc.
Alternatively, the surfaceness of insulated window is greater than 2um, and such as 2.8,3,3.53,4.85,5.83 etc.When corrosion-resistant coating is fine and close and thickness reaches more than 40um, the insulated window that roughness ratio is larger can have good adhesive power to corrosion-resistant coating.This is the increase due to insulated window surfaceness, add the contact area of interface zone between corrosion-resistant coating and matrix surface, corrosion-resistant coating contact area is become three-dimensional fragment (3-dimensionalfraction) from two-dimensional slices (2-dimensionalfraction).Deposition corrosion-resistant coating on uneven surface can cause the formation of coating random crystal orientation, and cause the release of the interfacial stress between corrosion-resistant coating and insulated window 204 matrix, which enhance the adsorptive power of insulated window 204 matrix and corrosion-resistant coating, and facilitate and thickly to be formed thereon with coating that is densification.
Further, when described corrosion-resistant coating has multilayered structure, described manufacture method also comprises the steps:, after performing thermal anneal processing step to the insulated window 204 being coated with corrosion-resistant coating, to carry out surface finish or milled processed to the corrosion-resistant coating of the multilayered structure on insulated window.The finishing of mating surface roughness and the formation of multilayered structure, the plasma body corrosion-resistant coating with higher caliper can be deposited on insulated window to strengthen interfacial adhesion.The roughness reducing surface can help to reduce the polymer deposition in manufacturing process process, therefore, it is possible to reduce metallic pollution.Typically, the surface of described insulated window can need to have specific roughness by the mode of grinding or polishing according to technique, is preferably below 0.1um.Alternatively, by suspension cleaning (slurrycleaning), atomization clean (aerosolcleaning), blast (blasting), roughened is carried out to corrosion-resistant coating or insulated window surface.Above-mentioned coarse surface treatment can repair the deposition on insulated window surface, to reduce the particle contamination in etching processing procedure.Above-mentioned polishing or the surface treatment step such as grinding or roughened can need to carry out before thermal anneal step or afterwards according to technique.
Further, the temperature span utilizing enhancement type physics or chemical vapour deposition to manufacture corrosion-resistant coating is for DEG C even higher higher than room temperature to 300.Wherein, it is all adjustable that the technological coefficient of enhancement type physics or chemical vapour deposition comprises temperature, pressure, power, it is adjusted to the corrosion-resistant coating forming good adhesion, also forming corrosion-resistant coating is alternatively smooth or uneven surface, and also forming etch resistant layer is alternatively single or multilayered structure.
Further, the present invention can also perform treatment step again being coated with on the insulated window 204 of corrosion-resistant coating, and to make improve its work-ing life, cost reduces.One of them again treatment step be mechanical workout insulated window 204 surface.Treatment step performs on used insulated window again, wherein, the surface of this insulated window 204 is in plasma damage mistake, or the settling institute of the coating on its surface in plasma etching processing procedure is overlapping or pollute, therefore perform this insulated window 204 again processed and can use the longer time, its production cost obtains reduction.
Further, described corrosion-resistant coating has different surface characteristic, such as, set specific surfaceness and make thick and the corrosion-resistant coating of densification can with good adhesion on insulated window.Above-mentioned having carried out also can correspondingly be extended the work-ing life being coated with the insulated window of corrosion-resistant coating that multiple coating or polishing obtain.
In detail thermal anneal step and technique effect thereof will be introduced below.Be the curve principle schematic of the thermal anneal step of the manufacture method of the insulated window of a kind of erosion-resisting jigger coupling type plasma process chamber according to the present invention's specific embodiment see Fig. 6, Fig. 6, its abscissa representing time, ordinate zou represents temperature.As shown in the figure, the insulated window 204 of the jigger coupling type plasma process chamber made for yttrium oxide is processing assembly, first insulated window 204 is sent into thermal annealing stove, within the t1 time period, with the speed of 2 DEG C or min, the temperature of insulated window 204 is elevated to 400 DEG C, then in following 3 hours, insulated window 204 is remained on 400 DEG C, finally within the t2 time period, with the speed of 1 DEG C or min, the temperature of insulated window 204 is reduced to 0.It should be noted that, t1 and the t2 time period only schematically shows for some time here, the concrete data of t1 and t2 are also not particularly limited, as long as the temperature of insulated window 204 is raised or the speed control that reduces within the specific limits, and finally reach top temperature or be reduced to 0 just passable.
It will be appreciated by those skilled in the art that the design parameter requirement that thermal anneal step performs, comprise time, top temperature, heat-up rate, cooling rate etc. and all decided by concrete material and the number of plies thereof.Fig. 7 is the parameter list of thermal anneal step for different material layer of the manufacture method of the insulated window of a kind of erosion-resisting jigger coupling type plasma process chamber according to the present invention's specific embodiment.As shown in the form of Fig. 7 signal, the Al after Material selec-tion is anodizing, require that the thickness that it is finally formed is 75um, when the number of plies is 1 layer, thermal anneal step needs to remain on 200 DEG C and reaches 4h.Before execution thermal anneal step, its initial stress is 3.27GPa, is 2.71 performing the follow-up stress after thermal anneal step, and its stress reduces amplitude and reaches 17%.When Material selec-tion is Al
2o
3, require that the thickness that it is finally formed is 75um, when the number of plies is 4 layers, thermal anneal step needs to remain on 400 DEG C and reaches 3h.Before execution thermal anneal step, its initial stress is 3.13GPa, is 2.24 performing the follow-up stress after thermal anneal step, and its stress reduces amplitude and reaches 28%.When Material selec-tion is Al, require that the thickness that it is finally formed is 90um, when the number of plies is 2 layers, thermal anneal step needs to remain on 200 DEG C and reaches 4h.Before execution thermal anneal step, its initial stress is 1.97GPa, is 1.71 performing the follow-up stress after thermal anneal step, and its stress reduces amplitude and reaches 13%.When Material selec-tion is Al, require that the thickness that it is finally formed is 130um, when the number of plies is 4 layers, thermal anneal step needs to remain on 200 DEG C and reaches 4h.Before execution thermal anneal step, its initial stress is 3.82GPa, is 2.53 performing the follow-up stress after thermal anneal step, and its stress reduces amplitude and reaches 34%.As can be seen here, the stress reduction of the thermal anneal step that the inventive method provides to various material all has unusual effect, which illustrates superiority of the present invention.
We also pass through Prague principle analysis STRESS VARIATION.Fig. 8 is Prague principle schematic, as shown in Figure 8, Prague principle is utilized to analyze the etch resistant layer d2 on the insulated window 204 of the jigger coupling type plasma process chamber utilizing the manufacture method of insulated window provided by the invention to obtain, particularly, from upper surface and the lower surface of incident at least two x-ray S11 and S21 to etch resistant layer d2 of the upper surface of etch resistant layer d2, obtain reflection ray S12 and diffracted ray S22 respectively through after reflection and diffraction.Therefore the x-ray of upper surface can reflect, and the x-ray of lower surface diffraction can occur.Wherein θ is diffraction angle (Bragg angle), and λ is X-ray wavelength, and 2d is crystal face distance, S=d*sin θ.According to Prague principle, if unstressed existence, under different angle Ψ (PSI), 2 θ angles, the crystal face of same (hkl) crystal face are unchanged apart from d.If there is unrelieved stress, under different angle Ψ (PSI), 2 θ angles, the crystal face of same (hkl) crystal face change apart from d with the change of inclination angle Ψ.If tensile stress, Ψ is larger, and d is larger.If stress, Ψ is larger, and d is less.If desirable plane stress state, then there is following relational expression:
σ=K·M
Wherein, E is Young's modulus, E=171.5GPa.V is Poisson's ratio, v=0.298.M be multiple deliver ψ condition under the change of same crystal face 2 θ value, carry out fitting of a straight line below and ask slope, slope is the M of above-mentioned relation formula.
Fig. 9 shows the graphic representation utilizing Prague principle fitting of a straight line to ask slope M, and its X-coordinate represents Sin
2ψ, ordinate zou is 2 θ, as shown in the figure, obtains its slope M=0.5614.Therefore, can learn, under different angle Ψ (PSI), 2 θ angles, the crystal face of same (hkl) crystal face are very little apart from d change, therefore illustrate that counter stress of the present invention reduction has unusual effect.
Although content of the present invention has done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple amendment of the present invention and substitute will be all apparent.Therefore, protection scope of the present invention should be limited to the appended claims.In addition, any Reference numeral in claim should be considered as the claim involved by restriction; " comprise " word and do not get rid of device unlisted in other claim or specification sheets or step; The word such as " first ", " second " is only used for representing title, and does not represent any specific order.
Claims (15)
1. the insulated window of an erosion-resisting jigger coupling type plasma process chamber, it is characterized in that: described insulated window utilizes plasma-enhanced physics or chemical vapour deposition at its coating of one side in the face of plasma body corrosion-resistant coating, described in be coated with corrosion-resistant coating insulated window carried out heat treatment step.
2. insulated window according to claim 1, is characterized in that: described heat treatment step comprises thermal anneal process.
3. insulated window according to claim 2, is characterized in that: the material of described etch resistant layer coating comprise following any one or appoint multiple: Y
2o
3, YF
3, ErO
2, Al
2o
3, SiC, AlN, ZrO
2.
4. insulated window according to claim 3, is characterized in that: the thickness of described corrosion-resistant coating is for being greater than 40um.
5. insulated window according to claim 3, is characterized in that: described etch resistant layer coating has multilayered structure.
6. insulated window according to claim 2, is characterized in that: the ceramic matrix of described insulated window is quartz or aluminum oxide.
7. a manufacture method for the insulated window of erosion-resisting jigger coupling type plasma process chamber, it is characterized in that, described manufacture method comprises the steps:
One insulated window matrix is provided;
Described insulated window matrix utilize enhancement type physics or chemical vapour deposition apply one deck corrosion-resistant coating in its one side in the face of plasma body;
Then heat treatment step is performed to the insulated window being coated with corrosion-resistant coating.
8. manufacture method according to claim 7, is characterized in that: described heat treatment step comprises thermal anneal process.
9. manufacture method according to claim 8, it is characterized in that, described manufacture method also comprises the steps: that one side insulated window being exposed to plasma body carries out roughened step, on described insulated window matrix, then utilize enhancement type physics or chemical vapour deposition to apply one deck corrosion-resistant coating in its one side in the face of plasma body.
10. manufacture method according to claim 9, is characterized in that: described roughened makes the surfaceness of insulated window be less than 0.5um.
11. manufacture method according to claim 9, is characterized in that: described roughened makes the surfaceness of insulated window be greater than 2um.
12. manufacture method according to claim 8, it is characterized in that, when described corrosion-resistant coating has multilayered structure, described manufacture method also comprises the steps:, after performing thermal anneal processing step to the insulated window being coated with corrosion-resistant coating, to carry out surface finish or milled processed to the corrosion-resistant coating of the multilayered structure on insulated window.
13. manufacture method according to claim 8, is characterized in that: the temperature span utilizing enhancement type physics or chemical vapour deposition to manufacture corrosion-resistant coating is higher than room temperature.
14. manufacture method according to claim 8, is characterized in that: the thickness of described corrosion-resistant coating is for being greater than 40um.
15. manufacture method according to claim 8, it is characterized in that: when described corrosion-resistant coating has multilayered structure, the Thickness scope of the every one deck single layer structure in its multilayered structure is 0.1um to 30um, and the number of multilayered structure can reach 1 to 100 layers.
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