CN111254417A - Memory manufacturing device and manufacturing method - Google Patents

Memory manufacturing device and manufacturing method Download PDF

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Publication number
CN111254417A
CN111254417A CN202010140903.5A CN202010140903A CN111254417A CN 111254417 A CN111254417 A CN 111254417A CN 202010140903 A CN202010140903 A CN 202010140903A CN 111254417 A CN111254417 A CN 111254417A
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CN
China
Prior art keywords
type
gas
nozzles
distance
tray
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Pending
Application number
CN202010140903.5A
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Chinese (zh)
Inventor
涂飞飞
王新胜
王雄禹
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Yangtze Memory Technologies Co Ltd
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Yangtze Memory Technologies Co Ltd
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Publication date
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Priority to CN202010140903.5A priority Critical patent/CN111254417A/en
Publication of CN111254417A publication Critical patent/CN111254417A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical 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
    • C23C16/455Chemical 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
    • C23C16/45563Gas nozzles
    • C23C16/45574Nozzles for more than one gas
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical 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
    • C23C16/50Chemical 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 using electric discharges
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005Apparatus not specifically provided for elsewhere
    • H01L21/67011Apparatus for manufacture or treatment

Abstract

The embodiment of the disclosure discloses a memory manufacturing device and a manufacturing method, wherein the device comprises: a cavity; the tray is positioned in the containing cavity; one or more first type nozzles located within the chamber; one or more second type nozzles located within the chamber; wherein the first type of nozzles are configured such that a first distance between the gas orifices and the center of the tray is a first distance, and the second type of nozzles are configured such that a distance between the gas orifices and the center of the tray is a second distance; the second distance is a numerical value, and the second distance is smaller than the first distance; or the second type of nozzles are movable nozzles, so that the second distance is a combination of a plurality of values or a numerical range, and the minimum value of the second distance is smaller than the first distance; the first type of nozzle and the second type of nozzle are used for spraying first gas.

Description

Memory manufacturing device and manufacturing method
Technical Field
The disclosed embodiments relate to the field of semiconductor technologies, and in particular, to a memory manufacturing apparatus and a memory manufacturing method.
Background
In the memory manufacturing process, a vapor deposition process is usually used to introduce gas into a chamber containing a target to form a thin film on the surface of the target.
Since the uniformity of the formed thin film directly affects the performance of the memory, how to improve the uniformity of the finally formed thin film is an urgent problem to be solved.
Disclosure of Invention
In view of the above, the present disclosure provides a memory manufacturing apparatus and a memory manufacturing method.
According to a first aspect of the embodiments of the present disclosure, there is provided a memory manufacturing apparatus, including:
a cavity;
the tray is positioned in the containing cavity;
one or more first type nozzles located within the chamber;
one or more second type nozzles located within the chamber;
wherein the first type of nozzles are configured such that the distance between the gas orifices and the center of the tray is a first distance, and the second type of nozzles are configured such that the distance between the gas orifices and the center of the tray is a second distance;
the second distance is a numerical value, and the second distance is smaller than the first distance; alternatively, the first and second electrodes may be,
the second type of nozzles are movable nozzles, so that the second distance is a combination of a plurality of values or a numerical range, and the minimum value of the second distance is smaller than the first distance; the first type of nozzle and the second type of nozzle are used for spraying first gas.
In some embodiments, a plurality of the first type of nozzles and a plurality of the second type of nozzles are distributed crosswise in a circumferential direction of the plenum.
In some embodiments, a plurality of nozzles of the first type are distributed in the cavity at equal angles in the circumferential direction with the center of the cavity as a symmetry center;
the second nozzles are distributed in the cavity at equal angles in the circumferential direction by taking the center of the cavity as a symmetrical center.
In some embodiments, the tray is a removable tray; the movable tray can rotate by taking the central shaft of the containing cavity as a rotating shaft.
In some embodiments, the apparatus further comprises:
a first gas supply tank for supplying the first gas;
the first type nozzles and the second type nozzles are communicated with the first air supply tank through first type air inlet pipes;
and a first type controlled valve for controlling the circulation of the first gas is arranged on the first type air inlet pipe.
In some embodiments, the apparatus further comprises:
the third type of nozzle is positioned in the cavity, is positioned in a vertical plane of a plane where the first type of nozzle and the second type of nozzle are positioned, and is used for spraying a second gas to the target object positioned on the tray;
wherein the second gas is capable of reacting with the first gas to form a thin film on the target surface.
In some embodiments, the apparatus further comprises:
a second gas supply tank for supplying the second gas;
the third type nozzle is communicated with a second air supply box through a second type air inlet pipe, and is connected with the third type nozzle, and a second type controlled valve for controlling the circulation of the second air is arranged on the second type air inlet pipe.
In some embodiments, the apparatus comprises a plasma vapor deposition apparatus;
the target includes a wafer.
In some embodiments, the number of the plurality of first type nozzles is an even number;
the number of the plurality of second type nozzles is even.
According to a second aspect of the embodiments of the present disclosure, there is provided a method for manufacturing a memory, including:
placing the target on a tray;
spraying a first gas to a first area of a tray, and spraying the first gas to a second area of the tray, wherein the concentration difference between the first gas in the first area and the first gas in the second area is within a preset range;
wherein a distance between the first region and the center of the tray is a first distance, a distance between the second region and the center of the tray is a second distance, and the first distance is not equal to the second distance.
In some embodiments, the placing the object on the tray comprises: fixing the target on the tray in the cavity;
the method further comprises the following steps: and the tray on which the target object is rotationally fixed is rotated by taking a central shaft of the cavity as a rotating shaft.
In some embodiments, the emitting the first gas to the first area of the tray and the emitting the first gas to the second area of the tray comprises:
and the first gas is sprayed to the first area through a first type of nozzle in the circumferential direction of the cavity for accommodating the target object, and the first gas is sprayed to the second area through a second type of nozzle in the circumferential direction of the cavity.
In some embodiments, a plurality of the first type of nozzles and a plurality of the second type of nozzles are distributed crosswise in a circumferential direction of the plenum.
When the distance that the first gas moves in the spraying direction increases after the first gas is sprayed from the nozzle, the moving speed of the first gas gradually decreases, and a part of the first gas can be adsorbed on the surface of the target object, so that when the moving distance of the first gas increases, the concentration of the first gas gradually decreases, resulting in different uniformity of the first gas on the surface of the target object.
Compared with the method that the first gas is sprayed to the surface of the target object through the nozzles with the same distance to the center of the tray, the memory manufacturing device provided by the embodiment of the disclosure sprays the first gas to the target object on the tray through the first type of nozzles and the second type of nozzles with different distances to the center of the tray, so that the distribution uniformity of the first gas on the surface of the target object and in the area with different distances to the center of the target object is improved, that is, the distribution uniformity of the first gas on the surface of the target object is improved, the uniformity of a thin film formed by using the first gas is improved, and the quality of the memory is improved.
Drawings
FIG. 1 is a schematic diagram illustrating a memory fabrication apparatus in accordance with an exemplary embodiment;
FIG. 2a is a schematic diagram illustrating an arrangement of a plurality of cavities according to an exemplary embodiment;
FIG. 2b is a schematic view of another arrangement of a plurality of cavities according to an exemplary embodiment;
FIG. 2c is a schematic view of yet another plurality of cavities shown in accordance with an exemplary embodiment;
FIG. 3 is a partial top view of a memory fabrication device shown in accordance with an exemplary embodiment;
FIG. 4a is a partial top view of another memory fabrication device shown in accordance with an exemplary embodiment;
FIG. 4b is a partial top view of yet another memory fabrication device, shown in accordance with an exemplary embodiment;
FIG. 4c is a partial top view of yet another memory fabrication device, shown in accordance with an exemplary embodiment;
FIG. 5 is a schematic diagram illustrating another memory fabrication apparatus in accordance with an illustrative embodiment;
FIG. 6 is a flow chart illustrating a method of fabricating a memory according to an exemplary embodiment;
FIG. 7a is a schematic diagram illustrating yet another memory fabrication apparatus in accordance with an illustrative embodiment;
FIG. 7b is a partial top view of yet another memory fabrication device, shown in accordance with an exemplary embodiment;
FIG. 8a is a schematic illustration of a film thickness profile according to an exemplary embodiment;
FIG. 8b is a schematic illustration of another film thickness distribution shown in accordance with an exemplary embodiment;
FIG. 9 is a schematic diagram illustrating yet another apparatus for fabricating a memory in accordance with an illustrative embodiment.
Detailed Description
The technical solutions of the present disclosure will be further explained in detail with reference to the drawings and examples. While exemplary implementations of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
The present disclosure is more particularly described in the following paragraphs with reference to the accompanying drawings by way of example. Advantages and features of the present disclosure will become apparent from the following description and claims. It is to be noted that the drawings are in a very simplified form and are not to precise scale, which is merely for the purpose of facilitating and distinctly claiming the embodiments of the present disclosure.
In the disclosed embodiment, the term "a is connected to B" includes A, B where a is connected to B in contact with each other, or A, B where a is connected to B in a non-contact manner with other components interposed between the two.
In the embodiments of the present disclosure, the terms "first", "second", and the like are used for distinguishing similar objects, and are not necessarily used for describing a particular order or sequence.
The technical means described in the embodiments of the present disclosure may be arbitrarily combined without conflict.
As shown in fig. 1, the present embodiment provides a memory manufacturing apparatus 100, including:
a chamber 101;
a tray 102 positioned within the cavity 101;
one or more first-type nozzles 110 located within the chamber 101;
one or more second type nozzles 120 located within the chamber 101;
wherein the first type nozzles 110 are arranged such that the distance between the gas nozzles and the center of the tray 102 is a first distance, and the second type nozzles 120 are arranged such that the distance between the gas nozzles and the center of the tray 102 is a second distance;
the second distance is a numerical value, and the second distance is smaller than the first distance;
alternatively, the first and second electrodes may be,
the second type nozzles 120 are movable nozzles, so that the second distance is a combination of a plurality of values or a range of values, and the minimum value of the second distance is smaller than the first distance;
a first type of nozzle 110 and a second type of nozzle 120 for emitting a first gas.
Illustratively, the apparatus 100 may comprise an apparatus for forming a thin film on a surface of a target by a vapor deposition process. For example, the apparatus 100 may comprise: a plasma vapor deposition apparatus, a chemical vapor deposition apparatus, or the like.
The apparatus 100 may further include means for purifying the target object by the gas. For example, the apparatus 100 may remove impurities such as particles attached to the surface of the object from the surface of the object by the flow of the first gas ejected from the first-type nozzle 110 and the second-type nozzle 120 to purify the object.
Illustratively, the apparatus 100 may include one or more cavities 101 therein, for example, 1, 2, 3, or 4 cavities 101 may be included. Each chamber 101 may have a tray 102, one or more first type nozzles 110, and one or more second type nozzles 120 disposed therein. It is understood that the plurality of cavities 101 in the apparatus 100 may be arranged arbitrarily.
Specifically, taking the example that the apparatus 100 includes 4 cavities 101, the 4 cavities 101 may be arranged in parallel at the same horizontal height as shown in fig. 2 a. Alternatively, the 4 chambers 101 may be arranged vertically as shown in fig. 2 b. Alternatively, some of the cavities 101 may be arranged horizontally, and another part of the cavities 101 may be arranged vertically, so as to form a multi-layered structure as shown in fig. 2 c.
The tray 102 provides a placement position of the object and also has a certain fixing function for the object. For example, the tray 102 may include: an electrostatic Chuck (ESC) for fixing a target by electrostatic adsorption; or, the chuck with the groove limits the sliding of the target object through the groove so as to fix the target object.
Illustratively, the shape of the tray 102 may include: has a shape with a center of symmetry. E.g. circular or circular, etc. The center of the tray 102 can be considered as the center of symmetry of the tray 102. For example, when the tray 102 is a circle, the center of the tray 102 is the center of the circle.
The target may include: and (5) a wafer. It is understood that the wafer may include: and a semiconductor substrate, such as a silicon substrate or a germanium substrate, of which the surface is not formed with the memory structure. The wafer may further include: the semiconductor substrate having a specific structure formed on the surface thereof is, for example, a substrate having a stacked structure formed thereon or a substrate having a transistor structure formed thereon.
It should be noted that when the object is placed on the tray 102 in parallel, a line connecting the center of the object and the center of the tray 102 is perpendicular to the plane of the tray 102. Here, the center of the target is the center of symmetry of the target. Specifically, when the target is a circular wafer, the center of the target is the center of the wafer.
Illustratively, when the apparatus 100 includes a plurality of second-type nozzles 120, the distance between the gas outlets of different second-type nozzles 120 and the center of the tray 102 may be the same, which facilitates uniform control of the different second-type nozzles 120 and reduces control difficulty.
Illustratively, when the apparatus 100 includes a plurality of second type nozzles 120, the distance between the gas orifices of different second type nozzles 120 and the center of the tray 102 may also be different.
When the distances between the gas outlets of the different second nozzles 120 and the center of the tray 102 are different, the different second nozzles 120 can respectively eject the first gas to the surface of the target and the areas with different distances from the center of the target, so that the control flexibility of the different second nozzles can be improved, the concentration of the first gas can be respectively controlled on the surface of the target and the areas with different distances from the center of the target, and the distribution uniformity of the first gas on the surface of the target can be improved.
Illustratively, the movable nozzle may include: a telescopic member; the telescopic part can change the value of the distance between the air outlet of the movable nozzle and the center of the tray 102 through the change of the length of the telescopic part, namely, the value of the second distance.
It should be noted that the nozzles 120 of different second types may also be all active nozzles when the distance between the gas outlets of the nozzles 120 of different second types and the center of the tray 102 is the same.
The first-type nozzle 110 and the second-type nozzle 120 may be the same in composition material, which may include: metal or plastic, etc.
FIG. 3 is a top view of a nozzle arrangement shown in accordance with an exemplary embodiment. Referring to fig. 3, when the distance that the first gas moves in the ejection direction increases after the first gas is ejected from the nozzle, the moving speed of the first gas gradually decreases, and a portion of the first gas may be adsorbed on the surface of the target. Therefore, the concentration of the first gas gradually decreases along the direction from the edge of the target to the center of the target, i.e., the uniformity of the first gas varies on the surface of the target.
It can be understood that when the first gas is used to deposit a thin film on a target surface, the uniformity of the first gas on the target surface may directly affect the uniformity of the formed thin film.
Compared with the method that the first gas is sprayed to the surface of the target object through the nozzles with the same distance to the center of the tray, the memory manufacturing device provided by the embodiment of the disclosure sprays the first gas to the target object on the tray through the first type of nozzles and the second type of nozzles with different distances to the center of the tray, so that the distribution uniformity of the first gas on the surface of the target object in the area with different distances to the center of the target object is improved, that is, the distribution uniformity of the first gas on the surface of the target object is improved, the uniformity of a thin film formed by the first gas is improved, and the quality of the manufactured memory is improved.
In some embodiments, the plurality of first-type nozzles 110 and the plurality of second-type nozzles 120 are distributed across the circumferential direction of the cavity 101.
It will be appreciated that the cavity 101 may comprise a cylindrical cavity and the circumferential direction of the cavity 101 may comprise the circumferential direction of the cylindrical cavity side wall.
Illustratively, one or more second-type nozzles 120 may be included between two adjacent first-type nozzles 110. Alternatively, one or more first-type nozzles 110 may be included between two adjacent second-type nozzles 120. Fig. 4a, 4b and 4c are each a partial schematic illustration of a top view of the apparatus 100 according to various exemplary embodiments. As can be seen from fig. 4a, 4b and 4c, the first-type nozzles 110 and the second-type nozzles 120 may be arranged on the sidewall of the chamber 101 in an intersecting manner.
In some embodiments, the plurality of first-type nozzles 110 are distributed in the chamber 101 at equal angles in the circumferential direction, with the center of the chamber 101 being a symmetry center;
the plurality of second-type nozzles 120 are distributed in the chamber 101 at equal angles in the circumferential direction with the center of the chamber 101 as a center of symmetry.
As can be seen from fig. 4a, 4b and 4c, when the number of the first nozzles 110 is different from that of the second nozzles 120, the angle between the adjacent first nozzles 110 and the center of the chamber 101 is different from the angle between the adjacent second nozzles 120 and the center of the chamber 101.
For example, when the target is a wafer, the number of the first type nozzles 110 may be an even number, and the number of the second type nozzles 120 may be an even number.
When the object is placed on the tray 102, the object is symmetrical about the center of the cavity 101. It can be understood that, in the embodiment of the present disclosure, by taking the center of the cavity 101 as a symmetry center, the plurality of first-type nozzles 110 are distributed in the cavity 101 at equal angles in the circumferential direction, and the plurality of second-type nozzles 120 are distributed in the cavity 101 at equal angles in the circumferential direction, which is beneficial to improving the distribution uniformity of the first gas sprayed from the first-type nozzles and the second-type nozzles on the surface of the target object.
In some embodiments, the tray 102 is a removable tray; the movable tray can rotate about the central axis of the chamber 101 as a rotation axis.
When the movable tray rotates about the central axis of the cavity 101, the object placed on the movable tray can rotate together with the movable tray and remain stationary relative to the movable tray.
It will be appreciated that the distance between the target surface area and the gas orifices of the first type of nozzle or the second type of nozzle has an effect on the concentration of the first gas in that area. The concentration of the first gas is greatest for the same first type of nozzle 110 in the region of the target surface directly below the first type of nozzle 110. Therefore, in the process of depositing the thin film by using the first gas, the movable tray carries the target to rotate by using the central axis of the cavity 101 as a rotating axis, which is beneficial to improving the distribution uniformity of the first gas on the surface of the target, and further improving the uniformity of the formed thin film.
In some embodiments, the apparatus 100 further comprises:
a first gas supply tank for supplying a first gas;
the first type nozzles 110 and the second type nozzles 120 are communicated with a first air supply tank through first type air inlet pipes;
a first type controlled valve for controlling the circulation of the first gas is arranged on the first type air inlet pipe.
The first type of controlled valve may include: manual valves, or automatic valves. The automatic valve may comprise an electrically controlled valve, a magnetically controlled valve, or the like.
The first type of controlled valve may comprise one or more controlled valves that can be used to open a path for the first gas flow or to close a path for the first gas flow. Alternatively, the first type of controlled valve may also be used to adjust the cross-sectional flow area for the first gas to flow through in order to control the flow rate of the first gas in the first type of inlet line.
For example, the first air supply tank may be in communication with the first type of nozzles via a first type of air inlet conduit, and the first air supply tank may be in communication with the second type of nozzles via a second first type of air inlet conduit. A first type controlled valve is arranged on a first type air inlet pipe, and a second first type controlled valve is arranged on a second first type air inlet pipe. Therefore, the circulation of the first gas in the first type of nozzles and the second type of nozzles can be controlled respectively, and the operation is flexible.
It can be understood that, in order to improve the distribution uniformity of the first gas on the surface of the target object, the flow rates of the first gas ejected from the first type nozzles and the second type nozzles to different areas of the target object can be ensured to be the same by controlling the gas ejection opening diameters of the first type nozzles and the second type nozzles, or the flow rates of the first gas in the first type nozzles and the second type nozzles, and the like.
For example, when the gas orifice diameter of the first-type nozzle 110 is different from the gas orifice diameter of the second-type nozzle 120, the flow rate of the first gas in the first-type nozzle 110 and the flow rate of the first gas in the second-type nozzle 120 may be controlled by different first-type controlled valves, respectively, so that the flow rate of the first gas at the gas orifice of the first-type nozzle 110 is the same as the flow rate at the gas orifice of the second-type nozzle 120.
Specifically, the flow rate of the first gas in the first-type nozzle 110 may be controlled by the first-type controlled valve, and the flow rate of the first gas in the second-type nozzle 120 may be controlled by the second first-type controlled valve, so that the flow rate of the first gas ejected toward the target object through the gas ejection port of the first-type nozzle 110 and the flow rate of the first gas ejected toward the target object through the gas ejection port of the second-type nozzle 120 may be the same.
For another example, when the gas orifice diameter of the first-type nozzle 110 is the same as that of the second-type nozzle 120, the flow rates of the first gas in the first-type nozzle 110 and the second-type nozzle 120 can be controlled by the same first-type controlled valve, so that the flow rate of the first gas ejected to the target object through the gas orifice of the first-type nozzle 110 is the same as the flow rate of the first gas ejected to the target object through the gas orifice of the second-type nozzle 120.
Alternatively, when the flow rate of the first gas in the first-type nozzles 110 is the same as the flow rate of the first gas in the second-type nozzles 120, the gas orifice diameter of the first-type nozzles 110 may be set to be the same as the gas orifice diameter of the second-type nozzles 120, so that the flow rate of the first gas at the gas orifice of the first-type nozzles 110 may be the same as the flow rate at the gas orifice of the second-type nozzles 120.
When the flow rate of the first gas in the first-type nozzle 110 and the flow rate of the first gas in the second-type nozzle 120 are respectively controlled by different first-type controlled valves so that the flow rate of the first gas in the first-type nozzle 110 is greater than the flow rate of the first gas in the second-type nozzle 120, the gas orifice diameter of the first-type nozzle 110 may be set to be smaller than the gas orifice diameter of the second-type nozzle 120, and thus, the flow rate of the first gas at the gas orifice of the first-type nozzle 110 may be the same as the flow rate at the gas orifice of the second-type nozzle 120.
In some embodiments, as can be seen from fig. 4a, 4b and 4c, when the plurality of first-type nozzles 110 are annularly distributed along the sidewall of the chamber and the plurality of second-type nozzles 120 are also annularly distributed along the sidewall of the chamber, the plurality of first-type nozzles 110 are used for spraying the first gas to the first region of the surface of the target, and the plurality of second-type nozzles 120 are used for spraying the first gas to the second region of the surface of the target. Here, the first region and the second region may be both annular regions, or the second region may also be a circular region, and the distance between the first region and the center of the target is greater than the distance between the second region and the center of the target.
Since the distance between the second type nozzles 120 and the center of the target is smaller than the distance between the first type nozzles 110 and the center of the target, the area of the first region may be larger than that of the second region. When the gas orifice diameter of the first-type nozzle 110 is the same as that of the second-type nozzle 120, in order to ensure uniformity of the thin film formed in the first region and the second region, the flow rates of the first-type nozzle 110 and the second-type nozzle 120 may be controlled by different first-type controlled valves, respectively, so that the density distribution of the first gas in the first region and the second region is the same.
In some embodiments, as shown with reference to fig. 5, the apparatus 100 further comprises:
a third type nozzle 130, which is positioned in the cavity 101 and in a vertical plane of the planes of the first type nozzle 110 and the second type nozzle 120, and is used for spraying a second gas to the target object positioned on the tray 102;
wherein the second gas is capable of reacting with the first gas to form a thin film on the target surface.
Since the first gas and the second gas may react to form the thin film, when the first gas and the second gas are sequentially ejected through the same nozzle, for example, when the first gas is ejected first and then the second gas is ejected through the same nozzle, a portion of the first gas may remain in the nozzle, and the remaining first gas may react with the second gas to form a solid thin film in the nozzle. Therefore, the cross-sectional area of the gas flow path in the nozzle may be reduced, which affects the flow rate of the nozzle, and even blocks the nozzle, so that the nozzle cannot be used to spray the first gas or the second gas subsequently, which is not favorable for ensuring the uniformity of the film.
Compared with the method that different reaction gases are respectively sprayed through the same nozzle, the first gas and the second gas are respectively sprayed into the cavity through different nozzles, so that the reaction probability of the reaction gases in the nozzle is reduced, the flow stability of the first gas or the second gas in the nozzle is ensured, and a foundation is laid for improving the uniformity of the surface film of the target.
In some embodiments, the apparatus 100 further comprises:
a second gas supply tank for supplying the second gas;
the third type nozzle 130 is communicated with the second gas supply tank through a second type gas inlet pipe, and the second type gas inlet pipe is connected with the third type nozzle 130 and is provided with a second type controlled valve for controlling the circulation of the second gas.
A second type of controlled valve may include: manual valves, or automatic valves. The automatic valve may comprise an electrically controlled valve, a magnetically controlled valve, or the like.
The second type of controlled valve may include one or more controlled valves that can be used to open or close the path for the second gas flow. Alternatively, the second type of controlled valve may also be used to adjust the cross-sectional flow area through which the second gas flows to control the flow rate of the second gas in the second type of inlet conduit.
FIG. 6 is a flow chart illustrating a method of fabricating a memory according to an example embodiment. Referring to fig. 6, the method includes the steps of:
s100: placing the target on a tray;
s110: spraying a first gas to a first area of a tray, and spraying the first gas to a second area of the tray, wherein the concentration difference between the first gas in the first area and the first gas in the second area is within a preset range;
the distance between the first area and the center of the tray is a first distance, the distance between the second area and the center of the tray is a second distance, and the first distance is not equal to the second distance.
Illustratively, the method can be applied to the memory manufacturing device provided by the embodiment of the disclosure.
The preset range of the concentration difference between the first gas in the first area and the first gas in the second area can include: the concentration difference between the first gas in the first region and the first gas in the second region is zero or extremely small.
It should be noted that, when the concentration difference between the first gas in the first region and the first gas in the second region is within the preset range, it can be considered that the concentration difference between the first gas in the first region and the first gas in the second region does not affect the thickness of the thin film deposited in the first region and the second region respectively by using the first gas; or the influence of the concentration difference on the thicknesses of the films respectively deposited in the first area and the second area by using the first gas is extremely small, so that the manufactured memory can meet the quality requirement.
It will be understood that when the first zone or the second zone is an annular zone, the distance between the annular zone and the centre of the tray is: this may be represented by the distance between the inner circle of the ring shape and the center of the tray, or may be represented by the distance between the outer circle of the ring shape and the center of the tray.
It is noted that the same way is used for defining the first distance and the second distance, when the first region and the second region may both be annular regions. For example, the first distance is represented by a distance between an inner circle of the first area and the center of the tray, and the second distance is represented by a distance between an inner circle of the second area and the center of the tray; alternatively, the first distance is represented by a distance between an outer circle of the first region and the center of the tray, and the second distance is represented by a distance between an outer circle of the second region and the center of the tray.
When the second area is a circular area, the second area covers the center of the tray, and the distance between the second area and the center of the tray can be represented by the distance between the circumference of the circular area and the center of the tray.
In the embodiment of the disclosure, the first gas is sprayed to the first area, and the first gas is sprayed to the second area, so that the concentration difference between the first gas in the first area and the first gas in the second area is within a preset range, the distribution uniformity of the first gas on the surface of the target object placed on the tray can be improved, the uniformity of a thin film formed by using the first gas can be improved, and the quality of the manufactured memory can be improved.
In some embodiments, S100 may comprise: fixing the target object on a tray in the cavity;
the method further comprises the following steps: the tray on which the target is fixed is rotated by using the central axis of the cavity as a rotating axis.
Illustratively, the central axis of the cavity is perpendicular to the plane of the tray, and the intersection point of the central axis of the cavity and the tray coincides with the center of the tray.
In practice, the first region and the second region may both be regions which are symmetrical about the central axis of the cavity.
According to the embodiment of the disclosure, the tray fixed with the target object is rotated by taking the central shaft of the cavity as the rotating shaft while the first gas is sprayed to the surface of the target object, so that the distribution uniformity of the first gas in the first area and the second area is improved, that is, the distribution uniformity of the first gas on the surface of the target object is improved, the uniformity of a thin film formed by using the first gas is improved, and the quality of the manufactured memory is improved.
In some embodiments, S110 may include:
the first gas is sprayed to the first area through a first type of nozzle in the circumferential direction of a cavity for accommodating a target object, and the first gas is sprayed to the second area through a second type of nozzle in the circumferential direction of the cavity.
When the target object is placed on the tray, the surface of the target object, which needs to be subjected to film deposition by using the first gas, is parallel to the plane of the circumferential direction of the cavity. In the embodiment of the disclosure, the first type of nozzles spray the first gas to the first area in the circumferential direction of the cavity, and the second type of nozzles spray the first gas in the circumferential direction of the cavity, so that the distribution uniformity of the first gas on the surface of the target object is improved.
In some embodiments, the plurality of nozzles of the first type and the plurality of nozzles of the second type are distributed crosswise in the circumferential direction of the plenum.
In the embodiment of the disclosure, the first gas is sprayed to the target object through the plurality of first-type nozzles and the plurality of second-type nozzles which are distributed in the circumferential direction of the cavity in a crossed manner, so that the distribution uniformity of the sprayed first gas on the surface of the target object is improved.
One specific example is provided below in connection with any of the embodiments described above:
example 1:
in the manufacturing process of the memory, the control of film thickness uniformity (with in wafer film non-uniformity control) on the wafer is an important index for evaluating the film deposition (film deposition) quality.
In the actual film manufacturing process, considering that the film formation usually needs to go through a plurality of process processes including the deposition process, only providing the optimized deposition process condition does not necessarily achieve the best film uniformity, but the process optimization can be achieved through the mutual coordination and complementation between two or more film process processes, so as to improve the uniformity of the finally formed film.
In the thin film deposition process, the film formation rate of a local area on the surface of a wafer is related to the number of particles for film formation which reach the local area of the wafer in a unit time. Specifically, the larger the number of particles for film formation that reach the local region of the wafer per unit time, the faster the film formation rate in the local region of the wafer.
Generally, a High Density Plasma (HDP) can be used to deposit a thin film on the surface of a target. For example, a dielectric thin film can be deposited on a target surface using a high-density plasma film forming apparatus provided by Applied Materials (AMAT).
In high-density plasma film formation, it is common to obtain the same number of positively charged particles and negatively charged particles by ionizing neutral particles to obtain plasma. For example, the plasma may be formed by means of capacitive coupling, or obtained by means of inductive coupling.
Referring to FIG. 7a, the plasma is ejected through nozzles in the sidewall and ceiling of the film forming apparatus toward the wafer surface. The arrows in fig. 7a are used to indicate the direction of movement of the plasma ejected from the nozzle.
Referring to fig. 7b, the plurality of nozzles disposed on the sidewall of the film forming apparatus shown in fig. 7a are spaced from the center of the wafer by the same distance and are uniformly distributed in the circumferential direction of the sidewall of the film forming apparatus, the plasma sprayed from the nozzles on the sidewall toward the surface of the wafer reaches the edge of the wafer first, and the plasma sprayed from the nozzles on the top reaches the center of the wafer first. In addition, the gas plasma sprayed from the side wall nozzle and the top nozzle moves in the space where the wafer is located and gradually covers the whole surface of the wafer so as to form a thin film on the surface of the wafer.
After the plasma is sprayed out of the nozzle, the moving speed of the plasma is gradually reduced, and partial plasma is adsorbed on the surface of the wafer, so that the number of the plasma on the surface of the wafer is gradually reduced along the moving direction of the plasma.
Specifically, when the plasma is sprayed from the nozzle on the sidewall of the film forming apparatus, the number of the plasma reaching the edge of the wafer is large, and the number of the plasma gradually decreases from the edge of the wafer to the center of the wafer, so that the plasma distribution on the surface of the wafer is not uniform, the thickness of the thin film formed on the surface of the wafer is not uniform, and the yield of the memory is affected.
In the related art, plasma may be ejected toward the center of the wafer through a nozzle at the top of the film forming apparatus so that the center of the wafer has sufficient plasma.
In the actual manufacturing process, after the thin film is deposited by using the high density plasma, the deposited thin film is also planarized by a Chemical Mechanical Polishing (CMP) process. The uniformity of the high density plasma deposited film directly affects the uniformity of the film formed after the cmp process.
Referring to fig. 7a, a coordinate system is formed by establishing an abscissa from the center of the wafer in a radial direction of the wafer and an ordinate in a film deposition direction perpendicular to the surface of the wafer, with the center of the wafer as an origin of coordinates. The abscissa is used to indicate the distance of the area where the thin film is deposited from the center of the wafer, and the ordinate is used to indicate the thickness of the deposited thin film.
Fig. 8a is a diagram illustrating a distribution of a thickness of a deposited thin film on a wafer surface before the thin film is deposited on the wafer surface by using the high density plasma and the deposited thin film is planarized by using the chemical mechanical polishing process using the film forming apparatus shown in fig. 7a and 7 b. FIG. 8b shows the film thickness distribution on the wafer surface after the high density plasma deposition and the CMP process to planarize the deposited film.
Referring to fig. 8a and 8b, the film deposited by the film forming apparatus shown in fig. 7a and 7b has a thickness between the center of the wafer and the edge of the wafer smaller than that of the wafer, and a thickness between the center of the wafer and the edge of the wafer smaller than that of the edge of the wafer, i.e., the thickness of the film from the center of the wafer to the edge of the wafer is distributed in a V shape.
It can be understood that, since the distance between the nozzle on the side wall and the wafer center is greater than the distance between the nozzle on the side wall and the wafer edge in fig. 7a, the plasma jetted from the nozzle on the side wall reaches the wafer edge first, and the plasma jetted from the nozzle on the top reaches the wafer center first, the number of the plasma on the wafer edge and the wafer center is sufficient, while the number of the plasma on the wafer center area (wafer middle zone) between the wafer center and the wafer edge is minimum, i.e. the gas density distribution in the wafer center area is weakest, so that the film thickness from the wafer center to the wafer edge will be distributed in a V shape, which makes the range of the film thickness to be removed by the subsequent chemical mechanical polishing process difficult to determine, and makes it difficult to ensure the quality of the manufactured memory.
Fig. 9 is a schematic diagram of a semiconductor fabrication apparatus 100 provided in this example. Referring to fig. 9, the apparatus 100 includes:
a chamber 101;
a tray 102 positioned within the cavity 101;
a plurality of first-type nozzles 110 positioned on a sidewall of the chamber 101;
a plurality of second-type nozzles 120 distributed across the sidewall of the chamber 101 with the plurality of first-type nozzles 110;
a third nozzle 130, disposed in the cavity 101 and in a vertical plane to the plane of the first-type nozzle 110 and the second-type nozzle 120, for spraying a second gas toward the target object disposed on the tray 102;
a first type of nozzle 110 and a second type of nozzle 120 for emitting a first gas to different areas of the target located on the tray 102;
wherein the first type nozzles 110 are arranged such that the distance between the gas nozzles and the center of the tray 102 is a first distance, and the second type nozzles 120 are arranged such that the distance between the gas nozzles and the center of the tray 102 is a second distance;
the second distance is a numerical value, and the second distance is smaller than the first distance;
alternatively, the first and second electrodes may be,
the second type nozzles 120 are movable nozzles such that the second distance is a combination of a plurality of values or a range of values, and the minimum value of the second distance is smaller than the first distance;
the second gas is capable of reacting with the first gas to form a thin film on the target surface.
Illustratively, the apparatus 100 may be used to form silicon dioxide (SiO) on a wafer surface2) A film. At this time, the first gas may include Silane (SiH)4) The second gas may include oxygen (O)2)。
The apparatus 100 may also include an energized coil for ionizing the first gas to produce a plasma of the first gas and for ionizing the second gas to produce a plasma of the second gas. Specifically, when the first gas comprises silane, ionizing the first gas may result in a plasma comprising silicon particles and hydrogen particles, and ionizing the second gas may result in a plasma comprising oxygen particles.
For example, the uniformity of the thin film formed on the wafer surface can be controlled by adjusting the sizes of the gas outlets of the first type nozzle 110, the second type nozzle 120 and the third type nozzle 130, or by adjusting the ratio of the gas ejected from the first type nozzle 110, the second type nozzle 120 and the third type nozzle 130.
In an actual manufacturing process, when a chemical mechanical polishing process is used to planarize a thin film, a polishing rate of the chemical mechanical polishing process to an edge of a wafer is generally higher than a polishing rate to a center of the wafer. Therefore, even if the film thickness uniformity satisfies the condition when the film is deposited, the uniformity of the film after polishing is poor due to the characteristics of the chemical mechanical polishing process itself. Therefore, it is generally necessary to set conditions for the corresponding thin film formation process in consideration of the characteristics of each process itself in the thin film formation process.
Compared with the first type of nozzles which are used for ejecting the first gas to the target object at the same distance with the center of the target object, the first type of nozzles which are partially arranged at the first distance with the center of the target object are replaced by the second type of nozzles which are arranged at the second distance with the center of the target object, wherein the first distance is different from the second distance, and the first gas is ejected to the surface of the wafer by the nozzles which are arranged at the different distances with the center of the target object, so that the adjusting capacity of the thickness of the film deposited on the surface of the target object is increased, and the uniformity of the formed film is improved. In addition, the method makes it possible to independently control the film thickness of different areas on the surface of the target object, and lays a foundation for providing customized film thickness distribution for the subsequent chemical mechanical polishing process.
In the embodiments provided in the present disclosure, it should be understood that the disclosed apparatus, system, and method may be implemented in other ways. The above description is only for the specific embodiments of the present disclosure, but the scope of the present disclosure is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present disclosure, and all the changes or substitutions should be covered within the scope of the present disclosure. Therefore, the protection scope of the present disclosure shall be subject to the protection scope of the claims.

Claims (13)

1. An apparatus for manufacturing a memory, comprising:
a cavity;
the tray is positioned in the containing cavity;
one or more first type nozzles located within the chamber;
one or more second type nozzles located within the chamber;
wherein the first type of nozzles are configured such that the distance between the gas orifices and the center of the tray is a first distance, and the second type of nozzles are configured such that the distance between the gas orifices and the center of the tray is a second distance;
the second distance is a numerical value, and the second distance is smaller than the first distance; alternatively, the first and second electrodes may be,
the second type of nozzles are movable nozzles, so that the second distance is a combination of a plurality of values or a numerical range, and the minimum value of the second distance is smaller than the first distance;
the first type of nozzle and the second type of nozzle are used for spraying first gas.
2. The apparatus of claim 1, wherein a plurality of said first type of nozzles and a plurality of said second type of nozzles are distributed across a circumferential direction of said plenum.
3. The apparatus of claim 2,
the first nozzles are distributed in the cavity at equal angles in the circumferential direction by taking the center of the cavity as a symmetrical center;
the second nozzles are distributed in the cavity at equal angles in the circumferential direction by taking the center of the cavity as a symmetrical center.
4. The apparatus of claim 1,
the tray is a movable tray; the movable tray can rotate by taking the central shaft of the containing cavity as a rotating shaft.
5. The apparatus of claim 1, further comprising:
a first gas supply tank for supplying the first gas;
the first type nozzles and the second type nozzles are communicated with the first air supply tank through first type air inlet pipes;
and a first type controlled valve for controlling the circulation of the first gas is arranged on the first type air inlet pipe.
6. The apparatus of claim 1, further comprising:
the third type of nozzle is positioned in the cavity, is positioned in a vertical plane of a plane where the first type of nozzle and the second type of nozzle are positioned, and is used for spraying a second gas to the target object positioned on the tray;
wherein the second gas is capable of reacting with the first gas to form a thin film on the target surface.
7. The apparatus of claim 6, further comprising:
a second gas supply tank for supplying the second gas;
the third type nozzle is communicated with a second air supply box through a second type air inlet pipe, and is connected with the third type nozzle, and a second type controlled valve for controlling the circulation of the second air is arranged on the second type air inlet pipe.
8. The apparatus of claim 1,
the apparatus comprises a plasma vapor deposition apparatus;
the target includes a wafer.
9. The apparatus of claim 1,
the number of the first type nozzles is even;
the number of the plurality of second type nozzles is even.
10. A method for fabricating a memory, comprising:
placing the target on a tray;
spraying a first gas to a first area of a tray, and spraying the first gas to a second area of the tray, wherein the concentration difference between the first gas in the first area and the first gas in the second area is within a preset range;
wherein a distance between the first region and the center of the tray is a first distance, a distance between the second region and the center of the tray is a second distance, and the first distance is not equal to the second distance.
11. The method of claim 10, wherein the placing the object on the tray further comprises:
fixing the target object on a tray in the cavity;
the method further comprises the following steps:
and the tray on which the target object is rotationally fixed is rotated by taking a central shaft of the cavity as a rotating shaft.
12. The method of claim 10, wherein ejecting the first gas toward the first region of the tray and ejecting the first gas toward the second region of the tray comprises:
the first gas is sprayed to the first area through a plurality of first type nozzles in the circumferential direction of a cavity containing the target object, and the first gas is sprayed to the second area through second type nozzles in the circumferential direction of the cavity.
13. The method of claim 12,
the plurality of nozzles of the first type and the plurality of nozzles of the second type are distributed in a crossed manner in the circumferential direction of the cavity.
CN202010140903.5A 2020-03-03 2020-03-03 Memory manufacturing device and manufacturing method Pending CN111254417A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6143078A (en) * 1998-11-13 2000-11-07 Applied Materials, Inc. Gas distribution system for a CVD processing chamber
US6383954B1 (en) * 1999-07-27 2002-05-07 Applied Materials, Inc. Process gas distribution for forming stable fluorine-doped silicate glass and other films
US20080095953A1 (en) * 2006-10-24 2008-04-24 Samsung Electronics Co., Ltd. Apparatus for depositing thin film and method of depositing the same
EP3610053A1 (en) * 2017-04-10 2020-02-19 Picosun Oy Uniform deposition
CN212426177U (en) * 2020-03-03 2021-01-29 长江存储科技有限责任公司 Memory manufacturing device

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6143078A (en) * 1998-11-13 2000-11-07 Applied Materials, Inc. Gas distribution system for a CVD processing chamber
US6383954B1 (en) * 1999-07-27 2002-05-07 Applied Materials, Inc. Process gas distribution for forming stable fluorine-doped silicate glass and other films
US20080095953A1 (en) * 2006-10-24 2008-04-24 Samsung Electronics Co., Ltd. Apparatus for depositing thin film and method of depositing the same
EP3610053A1 (en) * 2017-04-10 2020-02-19 Picosun Oy Uniform deposition
CN212426177U (en) * 2020-03-03 2021-01-29 长江存储科技有限责任公司 Memory manufacturing device

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
覃小红: "微纳米纺织品与检测", 东华大学出版社, pages: 29 *

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