CN110885970B - Pressure stabilizing and purifying device for solid precursor vapor and ALD deposition equipment - Google Patents
Pressure stabilizing and purifying device for solid precursor vapor and ALD deposition equipment Download PDFInfo
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- CN110885970B CN110885970B CN201811058058.6A CN201811058058A CN110885970B CN 110885970 B CN110885970 B CN 110885970B CN 201811058058 A CN201811058058 A CN 201811058058A CN 110885970 B CN110885970 B CN 110885970B
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- 239000002243 precursor Substances 0.000 title claims abstract description 89
- 239000007787 solid Substances 0.000 title claims abstract description 61
- 230000000087 stabilizing effect Effects 0.000 title claims abstract description 47
- 230000008021 deposition Effects 0.000 title claims abstract description 26
- 238000012545 processing Methods 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims description 34
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 239000012159 carrier gas Substances 0.000 claims description 13
- 239000011148 porous material Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 11
- 239000012712 low-vapor-pressure precursor Substances 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 description 27
- 238000000231 atomic layer deposition Methods 0.000 description 25
- 201000011452 Adrenoleukodystrophy Diseases 0.000 description 24
- 208000010796 X-linked adrenoleukodystrophy Diseases 0.000 description 24
- 239000010410 layer Substances 0.000 description 19
- 238000000034 method Methods 0.000 description 17
- 238000010438 heat treatment Methods 0.000 description 16
- 230000008569 process Effects 0.000 description 14
- 238000009826 distribution Methods 0.000 description 12
- 230000004888 barrier function Effects 0.000 description 11
- VSLPMIMVDUOYFW-UHFFFAOYSA-N dimethylazanide;tantalum(5+) Chemical compound [Ta+5].C[N-]C.C[N-]C.C[N-]C.C[N-]C.C[N-]C VSLPMIMVDUOYFW-UHFFFAOYSA-N 0.000 description 11
- 239000010408 film Substances 0.000 description 10
- 238000010926 purge Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 230000006641 stabilisation Effects 0.000 description 4
- 238000011105 stabilization Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 150000004820 halides Chemical class 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004070 electrodeposition Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 125000002524 organometallic group Chemical group 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- 239000011800 void material Substances 0.000 description 2
- 229910004546 TaF5 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910001502 inorganic halide Inorganic materials 0.000 description 1
- 239000002346 layers by function Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011165 process development Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- YRGLXIVYESZPLQ-UHFFFAOYSA-I tantalum pentafluoride Chemical compound F[Ta](F)(F)(F)F YRGLXIVYESZPLQ-UHFFFAOYSA-I 0.000 description 1
- GCPVYIPZZUPXPB-UHFFFAOYSA-I tantalum(v) bromide Chemical compound Br[Ta](Br)(Br)(Br)Br GCPVYIPZZUPXPB-UHFFFAOYSA-I 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
An embodiment of the present invention provides a pressure stabilizing and purifying apparatus for solid precursor vapor, including: a housing, wherein a closed processing space is formed inside the housing; the shell is provided with an air inlet and an air outlet which are communicated with the processing space; and a plurality of flow homogenizing members disposed inside the housing and sequentially arranged in a vertical direction, dividing the processing space into a plurality of subspaces sequentially arranged from bottom to top; the uniform flow component is provided with through holes, and adjacent subspaces are communicated through the through holes; wherein the air inlet is communicated with the subspace positioned at the lowest part; the exhaust port communicates with the uppermost subspace. An ALD deposition apparatus is also provided. The pressure stabilizing and purifying device can improve the stability of the vapor of the low vapor pressure precursor and reduce the pollution of the precursor solid particles to the conveying pipeline, the chamber and the product.
Description
Technical Field
Embodiments of the present invention relate to a pressure stabilizing and purifying apparatus for preparing a solid precursor vapor of TaN and an ALD deposition device.
Background
As semiconductor device dimensions enter the sub-micron age, cu acts as an interconnect metal due to low resistance (about 1.7 μΩ·cm, resistance of Al about 3.1 μΩ·cm), high current density, good thermal conductivity, and high electromigration resistance (higher electromigration resistance). These properties of Cu are more important as component wires below 22nm with high component density and speed. Cu is deposited in a relatively large number of ways, typically by PVD and ECD (electrochemical deposition). Since Cu diffuses into Si, siO2 and other low-k dielectric layer materials, the integrity of the component is easily destroyed, and the component is contaminated, it is important to deposit a good thin film of Ta/TaN or the like as a Cu diffusion barrier. In 22nm and below devices, a low-k dielectric PVD Ta/TaN barrier/PVD Cu seed layer/ECD Cu body stack is used. As the component size continues to decrease, the Cu diffusion barrier layer thickness is required to decrease to several nm. Currently, several metal nitride (TiN, taN, etc.) diffusion barriers are typically PVD deposited, but PVD methods have limited conformality of the deposited barrier film for structures with aspect ratios exceeding 2. In the high aspect ratio structure such as via, it is particularly critical to precisely control the thin film deposition process, especially the conformality of the barrier film within the interconnect structure. Conventional PVD or CVD processes are more challenging to deposit for an aspect ratio 5:1 diffusion barrier, resulting in void (void) formation due to directionality limitations. Especially in high density integrated Via structures, the aspect ratio is in the range of 5 to 10, even more than 10. The limitations of PVD or CVD processes in depositing high aspect ratio structures have therefore prompted the development of ALD processes and opened up new applications in this regard, requiring alternative methods for depositing barrier layers.
ALD exhibits unique advantages in high aspect ratio structures due to its uniformity and conformality over deposited nanoscale films. In fact, ALD deposits high aspect ratio structures are used in addition to the semiconductor industry for semi-gap dielectric layers for magnetic read and write heads, surface functional and protective layers for MEMS components, and the like.
The ALD process prepares TaN using precursors that typically include inorganic Ta halides and organometallic Ta compounds. Inorganic halide precursors include TaCl 5、TaF5、TaBr5、TaI5, employing NH 3 and N 2H4 as reactants. For the halide precursor, the prepared film is conductive and has good SC. However, when TaN is deposited as a barrier layer, a halogen element such as Cl present in the halogen compound of Ta will affect and corrode the subsequent deposition of the Cu layer film. In addition, ta is often deposited in a halide precursor of Ta xNy, and the high-valence Ta 3N5 film has a relatively high resistance value, which affects the performance requirements of the barrier film.
Some organometallic precursors of Ta are solid at room temperature and have low vapor pressure, and in addition to increasing the carrier gas, it is also necessary to increase the heating temperature by adding a heating function externally to increase the saturated vapor pressure of the source. Unlike liquid sources, solid sources cannot always remain level-parallel due to fluidity and gravity. The solid source is easier to evaporate in the heating process, and the part close to the edge of the source bottle is easier to evaporate than the part in the middle of the source bottle, so that the precursor vapor carried by the carrier gas inevitably contains solid particles in the process of heating and sublimating from the solid source to form vapor, and the solid particles enter a pipeline and a chamber to cause pollution; the difference in heating temperatures at the edge of the source bottle and the middle, upper and lower portions causes a difference in vaporization sublimation rate, and also inevitably causes instability of precursor vapor, thereby causing instability of the pulse number of the precursor in the ALD cycle pulse.
Disclosure of Invention
In order to solve at least one of the technical problems existing in the prior art, the embodiment of the invention provides a pressure stabilizing and purifying device for solid precursor vapor and ALD deposition equipment, so as to improve the stability of vapor of low vapor pressure precursor and reduce the pollution of precursor solid particles to a transmission pipeline, a chamber and products.
According to one embodiment of the present invention, there is provided a pressure stabilizing and purifying apparatus for solid precursor vapor, including:
a housing, wherein a closed processing space is formed inside the housing; the shell is provided with an air inlet and an air outlet which are communicated with the processing space; and
The uniform flow components are arranged inside the shell and are sequentially arranged along the vertical direction, and the processing space is divided into a plurality of subspaces which are sequentially arranged from bottom to top; the uniform flow component is provided with through holes, and adjacent subspaces are communicated through the through holes;
Wherein the air inlet is communicated with the subspace positioned at the lowest part; the exhaust port communicates with the subspace located at the uppermost portion.
In some examples, each flow homogenizing member extends in a horizontal direction and the plurality of flow homogenizing members are spaced apart in a vertical direction; the uniform flow component is provided with a plurality of through holes, and the through holes of adjacent uniform flow components are staggered.
In some examples, the air inlet and the air outlet are both disposed at a top of the housing; and a vent pipe is arranged in the shell, and vertically penetrates through the plurality of uniform flow components to communicate the air inlet with the subspace positioned at the lowest part.
In some examples, the housing includes a barrel and a cap; the top cover is detachably connected to the top of the cylinder body, and the air inlet and the air outlet are arranged on the top cover; one end of the vent pipe is connected to the position of the top cover corresponding to the air inlet.
In some examples, the flow-homogenizing member is a flow-homogenizing plate, the flow-homogenizing plate is disposed inside the cylinder, and an edge of the flow-homogenizing plate is connected to a side wall of the cylinder.
In some examples, the pressure stabilizing and purifying device for the solid precursor vapor further comprises a bushing, wherein two ends of the bushing are open, and the bushing is coaxially sleeved in the cylinder and is fit with the inner wall of the cylinder; the flow homogenizing component is a flow homogenizing plate; the flow-homogenizing plate is arranged inside the lining, and the edge of the flow-homogenizing plate is connected to the side wall of the lining.
In some examples, the vent tube is a straight tube, the air inlet and the vent tube being located on a vertical central axis of the housing; the apertures of the through holes are the same, and the number of the through holes gradually increases in a direction from the center of the flow homogenizing member to the edge of the flow homogenizing member.
In some examples, the vent tube is a straight tube, the air inlet and the vent tube being located on a vertical central axis of the housing; the through holes are uniformly distributed on the uniform flow member, and the aperture of the through holes is gradually increased in a direction from the center of the uniform flow member to the edge of the uniform flow member.
In some examples, the aperture of the through hole ranges from 1mm to 5mm.
According to another embodiment of the present invention, there is provided an ALD deposition apparatus including:
A source bottle containing a solid precursor therein;
the pressure stabilizing and purifying device for the solid precursor vapor adopts any one of the pressure stabilizing and purifying devices for the solid precursor vapor; and
A reaction chamber;
The inlet of the source bottle is connected with a carrier gas source, the outlet of the source bottle is connected with the pressure stabilizing and purifying device of the solid precursor vapor, and the pressure stabilizing and purifying device of the solid precursor vapor is connected with the reaction chamber.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the closed treatment space in the shell is divided into a plurality of subspaces which are sequentially arranged from bottom to top by arranging a plurality of uniform flow parts in the shell; the uniform flow component is provided with through holes, and adjacent subspaces are communicated through the through holes. The air inlet is communicated with the subspace positioned at the lowest part; the exhaust port communicates with the uppermost subspace. With this structure, the precursor vapor that enters the interior of the housing from the gas inlet first reaches the lowermost subspace, which forms the space for the source vapor storage. The precursor steam entering the shell sequentially passes through the through holes of the uniform flow parts from bottom to top, is gathered in subspaces of the corresponding layers layer by layer, and is finally discharged from the exhaust port, so that the stable supply flow of the precursor steam is realized, the steam pressure of the precursor is indirectly improved, the heating temperature of the precursor is not required to be improved, and the thermal decomposition of the precursor is avoided. Meanwhile, when particles in the precursor vapor flow through each layer of subspace, deposition and adsorption occur on the uniform flow plates of each layer due to the action of gravity, so that the deposition of the particles in the conveying pipeline, the spray head and the cavity is reduced.
The ALD deposition apparatus of the present invention includes the above-described pressure stabilizing and purifying device, and thus has the above-described advantages of the pressure stabilizing and purifying device as well.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following brief description of the drawings of the embodiments will make it apparent that the drawings in the following description relate only to some embodiments of the present invention and are not limiting of the present invention.
FIG. 1 is a schematic illustration of a portion of a circuit of an ALD deposition apparatus;
FIG. 2A is a schematic longitudinal cross-sectional view of a solid precursor vapor stabilization and purification apparatus according to an embodiment of the present invention;
FIG. 2B is a schematic longitudinal cross-sectional view of another apparatus for stabilizing and purifying a solid precursor vapor according to an embodiment of the present invention;
FIG. 3 is a schematic view of the structure of a top cover portion according to an embodiment of the present invention;
FIG. 4 is a schematic view of the structure of a barrel portion according to an embodiment of the present invention;
FIG. 5 is a schematic view of the structure of a flow homogenizing element according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of a portion of a circuit of an ALD deposition apparatus according to an embodiment of the present invention.
Reference numerals illustrate:
1-a reaction chamber; 2-gas distribution means; 3-a substrate; 4-heating the base; 5-pneumatic valve; 6-a vacuum pump; 7-source bottle; 8-a carrier gas and a purge gas; 9-a pressure stabilizing and purifying device for the solid precursor vapor; 10-a top cover assembly; 11-a cylinder; 12-a uniform flow component; 13-air inlet; 14-exhaust port; 15-a vent pipe; 16-top cover; 17-an annular shoulder; 18-a uniform flow plate; 19-a through hole; 20-the lowest subspace.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by a person skilled in the art without creative efforts, based on the described embodiments of the present invention fall within the protection scope of the present invention.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. The word "comprising" or "comprises", and the like, is intended to mean that elements or items preceding the word are included in the listed elements or items following the word, and equivalents thereof, without excluding other elements or items.
FIG. 1 is a schematic diagram of a portion of a circuit of an ALD deposition apparatus. The ALD deposition apparatus comprises a reaction chamber 1, a source bottle 7 for loading a precursor, and a vacuum pump 6. The bottom in the reaction chamber 1 is provided with the heating base 4, carries the substrate 3 on the heating base 4, and one side of reaction chamber 1 is provided with the pneumatic valve 5 that can let transmission device such as manipulator pass through in order to carry out the conveying to the substrate 3. A gas distribution device 2, namely a showcase, is provided in the top of the reaction chamber 1 opposite to the heating susceptor 4, and a reaction gas or a purge gas is introduced into the reaction chamber 1 through the gas distribution device 2. The bottom of the reaction chamber 1 is provided with an extraction opening, and a vacuum pump 6 is connected with the extraction opening and is used for extracting the gas in the reaction chamber 1. Taking the ALD deposition apparatus for depositing TaN as an example, the precursor loaded/contained in the source bottle 7 is pentakis (dimethylamino) tantalum (PDMAT), which is a solid source material for chemical vapor deposition or atomic layer deposition of highly conformal tantalum oxide or tantalum nitride films. The other precursor reaction source is ammonia (NH 3), and the precursor reaction source ammonia (NH 3) and connecting pipelines thereof are not shown in the figure. The reference numeral 8 in the figure indicates carrier gas and purge gas, and the carrier gas and the purge gas 8 are inert gases, and nitrogen is usually used. The source bottle 7 is provided with an inlet and an outlet, which are respectively connected with the carrier gas and the gas distribution device 2 in the reaction chamber 1 through pipelines, the gas distribution device 2 is also connected with the purge gas through pipelines, and the pipeline of the pumping hole of the reaction chamber 1 connected with the vacuum pump 6 is connected with the outlet of the source bottle 7 through a branch pipeline. The inlet of the source bottle 7 is connected with the connecting pipeline of the carrier gas and the outlet of the source bottle 7 is connected with the connecting pipeline of the gas distribution device 2 through two pipelines which are connected in parallel to form an H-shaped connecting pipe group. In the connecting pipelines shown in fig. 1, valves are arranged at corresponding positions according to the on-off requirements of the process flow on each pipeline, wherein PV 1-PV 6 are vacuum pneumatic valves 5, and MV1-MV 4 are manual valves; according to the requirements for the gas flow, mass flow controllers MFC1-MFC2 are arranged on the respective lines. The process steps of ALD deposition are known to those skilled in the art and will not be described in detail herein.
In the process of the ALD deposition apparatus shown in fig. 1, the precursor PDMAT is a solid precursor, the vapor pressure is low, and a heating device is usually arranged outside the source bottle 7 to heat the source bottle 7. Increasing the temperature can increase the amount of vapor, but can easily cause thermal decomposition of the precursor; the pressure of the PDMAT solid precursor vapor is low, and the flow fluctuation of the precursor vapor is large in the process of heating the precursor to sublimate and generate vapor; and the vapor generated by the solid precursor PDMAT is heated for sublimation, and particles which inevitably carry the precursor in the vapor generated in the sublimation process directly enter the conveying pipeline, the showcase and the cavity, so that pollution is caused and the purity of the deposited film is reduced.
In view of the above, embodiments of the present invention provide a pressure stabilizing and purifying device 9 for solid precursor vapor and an ALD deposition apparatus without increasing the complexity of piping and apparatus. According to one aspect of the present invention, as shown in fig. 2A and 2B, fig. 2A is a schematic longitudinal sectional view of a solid precursor vapor stabilization and purification apparatus 9 according to an embodiment of the present invention; fig. 2B is a schematic longitudinal cross-sectional view of another apparatus for stabilizing and purifying a solid precursor vapor according to an embodiment of the present invention. The device 9 for stabilizing and purifying the solid precursor vapor comprises a housing and a plurality of flow homogenizing members 12. The interior of the housing forms a closed process space. The shell is provided with an air inlet 13 and an air outlet 14 which are communicated with the processing space, and the air inlet 13 is used for enabling the processed gas to enter the processing space for processing; the exhaust port 14 is used to exhaust the processed gas in the processing space out of the processing space. The plurality of flow-homogenizing members 12 are disposed inside the housing, that is, the plurality of flow-homogenizing members 12 are located in the process space and are sequentially arranged in the vertical direction, dividing the process space into a plurality of subspaces sequentially arranged from bottom to top. The flow homogenizing member 12 is provided with through holes 19, and two adjacent subspaces are communicated through the through holes 19 so as to allow the processed gas to pass through.
Wherein the air inlet 13 communicates with the subspace 20 located at the lowermost portion; the exhaust port 14 communicates with the uppermost subspace. The flow direction of the gas to be processed in the processing space is from bottom to top in the vertical direction.
The flow-homogenizing member 12 may have a variety of different arrangements in the vertical direction inside the housing. Each of the flow-homogenizing members 12 may extend obliquely in a non-horizontal direction, and the oblique direction and angle of each of the flow-homogenizing members 12 may be different, and adjacent two of the flow-homogenizing members 12 may form partial contact at the edges. Each of the flow-homogenizing members 12 may also extend in the horizontal direction, and a plurality of the flow-homogenizing members 12 are arranged at intervals in the vertical direction. Other equivalent arrangements are also within the scope of the inventive concept.
Precursor vapor entering the interior of the housing from the inlet 13 first reaches the lowermost subspace 20, which forms the space for source vapor storage. The precursor steam entering the shell sequentially passes through the through holes 19 of the uniform flow parts 12 from bottom to top, is gathered in subspaces of the corresponding layers layer by layer, and is finally discharged from the exhaust port 14, so that the stable supply flow of the precursor steam is realized, the steam pressure of the precursor is indirectly improved, the heating temperature of the precursor is not required to be improved, and the thermal decomposition of the precursor is avoided. While particles in the precursor vapor are deposited and adsorbed on the flow-homogenizing plate 18 of each layer by gravity as they flow through the subspace of each layer, thereby reducing particle deposition in the transfer lines, showerhead and chamber. That is, the pressure stabilizing and purifying device 9 for solid precursor vapor of the present invention has the function of stabilizing and purifying the precursor vapor.
In some examples, each of the flow-homogenizing members 12 extends in a horizontal direction and a plurality of the flow-homogenizing members 12 are arranged at intervals in a vertical direction, and a plurality of through holes 19 are provided on each of the flow-homogenizing members 12. In order to improve the treatment effect, the through holes 19 between two adjacent uniform flow members 12 are arranged offset from each other. Therefore, a through channel between two non-adjacent subspaces is not formed in the flowing direction of the processed gas from the lowest subspace to the uppermost subspace, so that the residence time of the processed gas in each subspace layer can be increased, and the effects of better pressure stabilization and full precipitation of particles are achieved.
In some examples, each of the flow-homogenizing members 12 extends obliquely in a non-horizontal direction, and the oblique directions of adjacent two of the flow-homogenizing members 12 are opposite, the oblique angles are the same, and the adjacent two of the flow-homogenizing members 12 are not in contact. Each of the uniform flow members 12 is provided with a plurality of through holes 19. In order to improve the treatment effect, projections of the through holes 19 between two adjacent uniform flow members 12 on the horizontal plane are staggered, so that no through passage between two non-adjacent subspaces is formed in the flow direction of the treated gas.
In some examples, as shown in fig. 2A, both the intake port 13 and the exhaust port 14 are disposed at the top of the housing. Inside the housing is a vent pipe 15, the vent pipe 15 passing through the plurality of flow homogenizing members 12 in the vertical direction to communicate the air inlet 13 with the subspace 20 located at the lowermost portion. The provision of both the inlet 13 and the outlet 14 at the top of the housing facilitates the connection and arrangement of the piping when the pressure stabilizing and purifying device 9 for the solid precursor vapor is connected to the ALD deposition apparatus. As shown in fig. 2B, the air inlet 13 may be provided at the lower side or bottom of the housing, so that the air inlet 13 directly communicates with the lowermost subspace 20, and the vent pipe 15 is not required, thereby simplifying the structure.
In some examples, the housing may be a unitary structure or a split structure formed by connecting and combining multiple components. The plurality of flow homogenizing members 12 may be fixedly connected to the housing or may be detachably installed in the housing to facilitate replacement.
In some examples, the flow homogenizing member 12 may employ a disk-shaped flow homogenizing plate 18, or may employ other equivalent structures having similar shut-off and communication functions as the flow homogenizing plate 18, such as a flow homogenizing structure assembly composed of a plurality of members.
The technical scheme of the invention is further described and illustrated below according to some embodiments of the invention.
Example 1
With further reference to fig. 3 to 5, fig. 3 is a schematic structural view of a top cover part according to an embodiment of the present invention; fig. 4 is a schematic structural view of a portion of the cylinder 11 according to an embodiment of the present invention; fig. 5 is a schematic structural view of the flow-homogenizing member 12 according to an embodiment of the present invention. The housing of the pressure stabilizing and purifying device 9 for the solid precursor vapor comprises a cylinder 11 and a top cover 16. The cylinder 11 is cylindrical, the bottom of the cylinder 11 is closed, and the upper end is open. A disc-shaped top cover 16 is detachably connected to the top of the cylinder 11, and an air inlet 13 and an air outlet 14 are formed in the top cover 16. One end of the ventilation pipe 15 is connected to the inside of the top cover 16 (the side facing the inside of the cylinder 11) at a position corresponding to the air inlet 13, and may be screwed or welded. The outer side of the top cover 16 (the side facing the outside of the cylinder 11) is connected with pipe joints corresponding to the air inlet 13 and the air outlet 14, so as to be convenient to quickly detach or connect with the air inlet pipeline and the air outlet pipeline. Referring to fig. 3, the top cover 16, the pipe joints at the air inlet 13 and the air outlet 14, and the ventilation pipe 15 are connected to form an integral unit (hereinafter referred to as a top cover assembly 10) to facilitate connection and disconnection with the cylinder 11.
Referring to fig. 5, the flow homogenizing member 12 adopts disc-shaped flow homogenizing plates 18, the flow homogenizing plates 18 are arranged at intervals along the vertical direction, each flow homogenizing plate 18 is horizontally arranged, a cylindrical bushing is arranged around a plurality of flow homogenizing plates 18, two ends of the bushing are open, and the bushing is coaxially sleeved in the cylinder 11 and is attached to the inner wall of the cylinder 11, namely, the outer side of the side wall of the bushing is detachably attached to the inner side of the side wall of the cylinder 11. The edges of the flow-homogenizing plate 18 are attached to the side wall of the bushing, for example by fixing the edges of the flow-homogenizing plate 18 from outside the side wall of the bushing by screws, or by directly welding the edges of the flow-homogenizing plate 18 to the side wall of the bushing. Referring to fig. 4, to facilitate positioning of the uniform flow plate 18 and liner formed integrally within the barrel 11, an annular shoulder 17 is formed on the inside of the sidewall of the lower portion of the barrel 11 with the shoulder surface facing upward, a distance from the bottom of the barrel 11. The diameter of the bushing is larger than the inner diameter of the annular shoulder 17 so that the bottom of the bushing rests on the annular shoulder 17. After the integrated body of the flow-homogenizing plate 18 and the liner is placed and positioned in the drum 11, a lowermost subspace 20, i.e. a space in which the source steam is stored, is formed between the lowest flow-homogenizing plate 18 and the bottom of the drum 11.
Referring to fig. 2A, the vent pipe 15 is a straight pipe, and the air inlet 13 and the vent pipe 15 are located on the vertical central axis of the cylinder 11. The center of each flow homogenizing plate 18 is provided with a perforation through which the vent pipe 15 passes. After the flow homogenizing plate 18 and the bushing are installed, the vent pipe 15 in the top cover assembly 10 is extended to the lowest subspace 20 through the perforation of the flow homogenizing plate 18. Since the source steam enters from the straight-through pipe in the center of the device, the steam pressure in the middle part is high, so that the through holes 19 are designed according to the pressure and the distribution characteristics of the air flow. For example, the apertures of the through holes 19 on each of the uniform flow plates 18 are the same, and the number of through holes 19 distributed on the circumference of the same radius gradually increases in the direction from the center of the uniform flow plate 18 to the edge of the uniform flow plate 18. Or the through holes 19 on each of the flow-equalizing plates 18 are uniformly distributed on the flow-equalizing plates 18, and the aperture of the through holes 19 is gradually increased in a direction from the center of the flow-equalizing plate 18 to the edge of the flow-equalizing plate 18. Wherein the aperture of the through hole 19 is in the range of 1mm-5mm, preferably 3mm.
The detachable structure adopted in this embodiment can separate the three parts of the device very conveniently according to the need, and the uniform flow component 12 of the device is taken out from the cylinder 11 and then cleaned for reuse, so that the detachable structure is convenient to install after cleaning and is directly placed on the annular shoulder 17 in the cylinder 11.
Example two
The present embodiment provides a pressure stabilizing and purifying device 9 for solid precursor vapor, which is different from the embodiment in the structure: no bushing is provided and no annular shoulder 17 is required in the barrel 11. The disc-shaped uniform flow plates 18 are arranged in the barrel 11 at intervals along the vertical direction, and edges of the uniform flow plates 18 are connected to the side wall of the barrel 11. The edge of the flow-homogenizing plate 18 can be fixedly connected from the outer side of the side wall of the cylinder 11 by a screw, or the edge of the flow-homogenizing plate 18 can be directly welded on the side wall of the cylinder 11.
Example III
The present embodiment provides a pressure stabilizing and purifying device 9 for solid precursor vapor, which is different from the embodiment in the structure: the disc-shaped flow homogenizing plates 18 are arranged in the inside of the cylinder 11 at intervals in the vertical direction, the vent pipe 15 passes through the perforations of the flow homogenizing plates 18, and each flow homogenizing plate 18 is fixedly connected with the vent pipe 15 at the perforation. The liner can be arranged in the cylinder 11 or not, if the liner is not arranged, the diameter of the uniform flow plate 18 is slightly smaller than the inner diameter of the cylinder 11, and the annular shoulder 17 is not required to be arranged in the cylinder 11; if a bushing is provided, the diameter of the uniform flow plate 18 is slightly smaller than the inner diameter of the bushing. When disassembled, the flow-homogenizing plate 18 can be removed at the same time as the header assembly 10 is removed. The flow homogenizing plate 18 can be connected to the vent pipe 15 through threads, or can be directly welded to the vent pipe 15.
Example IV
The embodiment provides an ALD deposition device, and optimizes the mode of leading the sublimated vapor of the PDMAT source bottle 7 into a cavity. Referring to FIG. 6, FIG. 6 is a schematic diagram of a portion of an ALD deposition apparatus according to an embodiment of the invention. The ALD deposition apparatus is used for depositing TaN barrier layers, comprising a source bottle 7, a steady pressure and purification device 9 for solid precursor vapor and a reaction chamber 1. The source vial 7 contains a solid precursor, such as PDMAT. The pressure stabilizing and purifying device 9 for solid precursor vapor may employ the pressure stabilizing and purifying device 9 for various solid precursor vapors described in the first to third embodiments. The inlet of the source bottle 7 is connected with a carrier gas source, the outlet of the source bottle 7 is connected with a pressure stabilizing and purifying device 9 of the solid precursor vapor, and the pressure stabilizing and purifying device 9 of the solid precursor vapor is connected with the reaction chamber 1. That is, in this embodiment, a source PDMAT vapor treatment device is added after the outlet of the PDMAT source bottle 7, specifically, a heating base 4 is disposed at the bottom of the reaction chamber 1, a substrate 3 is carried on the heating base 4, and a pneumatic valve 5 capable of allowing a transfer device such as a manipulator to pass through to transfer the substrate 3 is disposed at one side of the reaction chamber 1. A gas distribution device 2, namely a showcase, is provided in the top of the reaction chamber 1 opposite to the heating susceptor 4, and a reaction gas or a purge gas is introduced into the reaction chamber 1 through the gas distribution device 2. The bottom of the reaction chamber 1 is provided with an extraction opening, and a vacuum pump 6 is connected with the extraction opening and is used for extracting the gas in the reaction chamber 1. The carrier gas and purge gas 8 employed was nitrogen. The source bottle 7 is provided with an inlet and an outlet, which are respectively connected with the carrier gas and the gas distribution device 2 in the reaction chamber 1 through pipelines, the gas distribution device 2 is also connected with the purge gas through pipelines, and the pipeline of the pumping hole of the reaction chamber 1 connected with the vacuum pump 6 is connected with the outlet of the source bottle 7 through a branch pipeline. The inlet of the source bottle 7 is connected with the connecting pipeline of the carrier gas and the outlet of the source bottle 7 is connected with the connecting pipeline of the gas distribution device 2 through two pipelines which are connected in parallel to form an H-shaped connecting pipe group. A pressure stabilizing and purifying device 9 for the solid precursor vapor is connected to a downstream pipeline connected to the outlet of the source bottle 7, and the precursor vapor flowing out of the source bottle 7 is subjected to pressure stabilizing and purifying treatment. Valves are arranged at corresponding positions according to the on-off requirements of the technological process on each pipeline, wherein PV 1-PV 6 are vacuum pneumatic valves 5, and MV1-MV 4 are manual valves; according to the requirements for the gas flow, mass flow controllers MFC1-MFC2 are arranged on the respective lines.
Parts not described in the present embodiment may refer to corresponding parts in the first embodiment. Likewise, the beneficial technical effects of the stabilization and purification device 9 of the solid precursor vapor in the first embodiment can be obtained in the ALD deposition apparatus in the present embodiment.
The invention ensures the stable entry amount of the precursor gas into the cavity in the PDMAT source bottle 7 by providing the pressure stabilizing and purifying device 9 of the solid precursor vapor and the ALD deposition equipment, thereby improving the stability and self-restriction of the process; the probability of precursor particles entering the pipeline, the showcase and the chamber is reduced, and the purity of the film is increased. The PDMAT vapor can be stored at the pressure stabilizing and purifying device 9 of the solid precursor vapor, indirectly increasing the amount of stable saturated vapor entering the reaction chamber 1, which is significant for larger scale process development, especially industrial production.
The description of the above embodiments is not limiting, and any suitable technical solution in the art may be adopted for the components or arrangements not mentioned in the above embodiments. The technical features of the different embodiments of the present invention can be arbitrarily combined.
The foregoing is merely exemplary embodiments of the present invention and is not intended to limit the scope of the invention, which is defined by the appended claims.
Claims (10)
1. A pressure stabilizing and purifying device for solid precursor vapor, comprising:
a housing, wherein a closed processing space is formed inside the housing; the shell is provided with an air inlet and an air outlet which are communicated with the processing space; and
The uniform flow components are arranged inside the shell and are sequentially arranged along the vertical direction, and the processing space is divided into a plurality of subspaces which are sequentially arranged from bottom to top; the uniform flow component is provided with a through hole, adjacent subspaces are communicated through the through hole, and no through passage exists between two non-adjacent subspaces;
Wherein the air inlet is communicated with the subspace positioned at the lowest part; the exhaust port communicates with the subspace located at the uppermost portion.
2. The apparatus for stabilizing and purifying a solid precursor vapor according to claim 1, wherein each of the flow homogenizing members extends in a horizontal direction and a plurality of the flow homogenizing members are arranged at intervals in a vertical direction; the uniform flow component is provided with a plurality of through holes, and the through holes of adjacent uniform flow components are staggered.
3. The apparatus for stabilizing and purifying a solid precursor vapor of claim 1, wherein the gas inlet and the gas outlet are both disposed at the top of the housing; and a vent pipe is arranged in the shell, and vertically penetrates through the plurality of uniform flow components to communicate the air inlet with the subspace positioned at the lowest part.
4. The apparatus for stabilizing and purifying a solid precursor vapor of claim 3, wherein the housing comprises a barrel and a top cap; the top cover is detachably connected to the top of the cylinder body, and the air inlet and the air outlet are arranged on the top cover; one end of the vent pipe is connected to the position of the top cover corresponding to the air inlet.
5. The apparatus for stabilizing and purifying a solid precursor vapor according to claim 4, wherein the flow homogenizing means is a flow homogenizing plate, the flow homogenizing plate is disposed inside the cylinder, and an edge of the flow homogenizing plate is connected to a side wall of the cylinder.
6. The apparatus for stabilizing and purifying solid precursor vapor according to claim 4, wherein the apparatus for stabilizing and purifying solid precursor vapor further comprises a bushing, the bushing is opened at both ends, and the bushing is coaxially sleeved in the cylinder and is attached to the inner wall of the cylinder; the flow homogenizing component is a flow homogenizing plate; the flow-homogenizing plate is arranged inside the lining, and the edge of the flow-homogenizing plate is connected to the side wall of the lining.
7. A device for stabilizing and purifying a solid precursor vapor according to claim 3 wherein said vent tube is a straight-through tube, said air inlet and said vent tube being located on a vertical central axis of said housing; the apertures of the through holes are the same, and the number of the through holes gradually increases in a direction from the center of the flow homogenizing member to the edge of the flow homogenizing member.
8. A device for stabilizing and purifying a solid precursor vapor according to claim 3 wherein said vent tube is a straight-through tube, said air inlet and said vent tube being located on a vertical central axis of said housing; the through holes are uniformly distributed on the uniform flow member, and the aperture of the through holes is gradually increased in a direction from the center of the uniform flow member to the edge of the uniform flow member.
9. The apparatus for stabilizing and purifying a solid precursor vapor according to claim 7 or 8, wherein the pore diameter of the through-hole ranges from 1mm to 5mm.
10. An ALD deposition apparatus, comprising:
A source bottle containing a solid precursor therein;
A pressure stabilizing and purifying device for solid precursor vapor, which adopts the pressure stabilizing and purifying device for solid precursor vapor according to any one of claims 1 to 9; and
A reaction chamber;
The inlet of the source bottle is connected with a carrier gas source, the outlet of the source bottle is connected with the pressure stabilizing and purifying device of the solid precursor vapor, and the pressure stabilizing and purifying device of the solid precursor vapor is connected with the reaction chamber.
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| CN201811058058.6A CN110885970B (en) | 2018-09-11 | 2018-09-11 | Pressure stabilizing and purifying device for solid precursor vapor and ALD deposition equipment |
| TW108131834A TWI716998B (en) | 2018-09-11 | 2019-09-04 | Stabilization and purification device for solid precursor vapor and ALD deposition equipment |
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| CN201811058058.6A CN110885970B (en) | 2018-09-11 | 2018-09-11 | Pressure stabilizing and purifying device for solid precursor vapor and ALD deposition equipment |
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| CN113186513A (en) * | 2021-05-31 | 2021-07-30 | 聚灿光电科技（宿迁）有限公司 | Solid raw material source bottle and CVD device with same |
| CN114277358B (en) * | 2021-11-12 | 2023-10-27 | 北京北方华创微电子装备有限公司 | Liquid source bottle and semiconductor process equipment |
| CN113818012B (en) * | 2021-11-25 | 2022-04-01 | 新美光(苏州)半导体科技有限公司 | Chemical vapor deposition device |
| CN114086155B (en) * | 2022-01-18 | 2022-04-15 | 北京中科重仪半导体科技有限公司 | Gas nozzle |
| CN116103636A (en) * | 2023-04-12 | 2023-05-12 | 上海星原驰半导体有限公司 | Solid-phase precursor output device and vapor deposition system |
| CN117966127B (en) * | 2024-04-02 | 2024-06-25 | 常州容导精密装备有限公司 | Heat conduction structure of precursor source bottle and control method |
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