CN117602803A - A high-purity quartz diffuser and its preparation method - Google Patents
A high-purity quartz diffuser and its preparation method Download PDFInfo
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- CN117602803A CN117602803A CN202311622993.1A CN202311622993A CN117602803A CN 117602803 A CN117602803 A CN 117602803A CN 202311622993 A CN202311622993 A CN 202311622993A CN 117602803 A CN117602803 A CN 117602803A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
- C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
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- 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
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Abstract
The invention discloses a preparation method of a high-purity quartz diffuser, which comprises the following steps: step 1: preparing slurry; step 2: preparing a blank; step 3: forming a blank; step 4: volatilizing the organic foam on the surface of the blank after the firing forming; step 5: sintering the obtained blank at high temperature; step 6: annealing the sintered blank; step 7: and naturally cooling the annealed blank body to room temperature in a vacuum sintering furnace. The method adopts high-purity fumed silica, combines with a deionized water high-speed dispersion process to prepare a high-purity siliceous dispersing agent, and prepares slurry by matching the high-purity siliceous dispersing agent with high-purity nanoscale quartz particles, thereby ensuring the purity of raw materials; after the green body is formed, the multi-temperature section long heat preservation technology is adopted to effectively remove the organic foam and simultaneously prevent the green body from deforming, and the yield of the diffuser prepared by the method provided by the invention can reach more than 80%.
Description
Technical Field
The invention discloses the technical field of quartz device preparation, in particular to a high-purity quartz diffuser and a preparation method thereof.
Background
The wafer process requires multiple thin film depositions in the reaction chamber, and the thin film deposition process which is more commonly used at the present stage is Chemical Vapor Deposition (CVD) for short. At present, ventilation components in CVD chemical vapor deposition equipment for wafer manufacturing processes at home and abroad all adopt a mode of opening holes in the wall of a quartz glass tube, wherein the hole diameter is generally 1.0mm, and the hole spacing is 10-12mm. The gas is sprayed out through the small holes of the quartz glass tube under the action of pressure, gas phase chemical reaction occurs in the reaction chamber, and the solid reactant is uniformly deposited on the surface of the substrate to form a film. The purity of the quartz glass tube is required to be over 99.99999 percent in order to ensure the wafer manufacturing process.
In CVD chemical vapor deposition, gas is injected in a mode of opening a quartz tube wall, and the gas enters the reaction chamber in a beam-shaped airflow. The beam-shaped air flows have certain directivity and gaps exist among the air flows. The injection mode easily causes uneven dispersion of gas in the reaction chamber, and influences the quality of the film in the later stage.
Therefore, providing a high purity quartz diffuser to uniformly disperse the gases in the reaction chamber is a highly desirable problem. The method disclosed in the prior art has the following problems: if the granulation process of the granulation method is carried out by a granulation method, a large amount of introduced organic matters cannot be removed in the later period; VAD deposition is complex and difficult to control, and mass production is difficult to realize; the photo-curing forming method is easy to deform in the later lipid discharging process, low in yield and the like.
Disclosure of Invention
In view of the above, the present disclosure provides a high purity quartz diffuser and a method for preparing the same;
the technical scheme provided by the invention is that the preparation method of the high-purity quartz diffuser comprises the following steps:
step 1: preparing slurry: according to parts by weight, 30-40 parts of high-purity fumed silica is obtained, 60-70 parts of deionized water are mixed under the condition of high-speed dispersion to obtain a high-purity siliceous dispersing agent, and after standing, 35 parts of the high-purity siliceous dispersing agent and 65 parts of high-purity quartz micro powder are obtained and mixed under the condition of high-speed dispersion to obtain slurry;
step 2: preparing a blank: immersing the pretreated reticulated polyurethane foam into the slurry to fully and uniformly coat the slurry on the polyurethane foam;
step 3: and (3) blank forming: drying and molding the prepared green body within 120 min;
step 4: volatilizing the organic foam on the surface of the blank after the firing forming;
step 5: sintering the blank obtained in the step 4 at a high temperature;
step 6: annealing the sintered blank;
step 7: and naturally cooling the annealed blank body to room temperature in a vacuum sintering furnace.
Preferably, the total metal ion content in the high purity fumed silica is less than 50ppm; the conductivity of the deionized water is 16-18MΩ & cm;
the technological parameters of mixing the high-purity fumed silica and deionized water under the condition of high-speed dispersion are as follows: the rotating speed of the high-speed dispersing machine is 1600-1800r/min, the dispersing time is 120min, and the standing time after mixing is 3-5min;
the purity of the high-purity quartz micro powder is more than 99.99999 percent, and the granularity D 50 200-250nm；
The technological parameters of mixing the high-purity siliceous dispersing agent and the high-purity quartz micro powder under the condition of high-speed dispersion are as follows: the rotating speed of the high-speed dispersing machine is 200-300r/min, and the dispersing time is 30min.
Preferably, the slurry is coated on the polyurethane foam, comprising the following: after the pretreated reticular polyurethane foam is immersed into the slurry, repeatedly extruding the reticular polyurethane foam body for 8-10 times by adopting a PP material pressure head to apply 5N pressure, and then placing the reticular polyurethane foam and the slurry in a centrifuge for 500-600r/min, wherein the treatment time is 3-4min; and taking out the reticular polyurethane foam, placing the reticular polyurethane foam on a pp material filter screen, and removing redundant slurry on the reticular polyurethane foam by adopting pure compressed air.
Preferably, the method adopts pure compressed air to remove redundant slurry on the reticulated polyurethane foam, and comprises the following technological parameters: the air nozzle is 5-10cm away from the surface of the blank and perpendicular to the surface of the blank for ventilation for 2-3min, and is more than 1cm away from the edge of the net-shaped polyurethane foam of the blank, and the air pressure is 2.5Mpa.
Preferably, the pre-treated reticulated polyurethane foam: placing the reticulated polyurethane foam into an ultrasonic cleaning tank, cleaning for 30s, removing superfluous particles attached to the surface, cleaning with deionized water, placing into an oven, and baking for 30min, wherein the temperature of the oven is 50-55 ℃.
Preferably, the drying and molding of the obtained green body comprises: and (3) in a ventilation drying furnace, ventilating and drying for 60 minutes at the temperature of 100-150 ℃, and ventilating pure air upwards perpendicular to the lower surface of the blank.
Preferably, the heating program of the volatilizing and firing organic foam is as follows: in a vacuum sintering furnace, the temperature is kept for 1 hour under the condition that the room temperature is raised to 500 ℃ at the temperature rising rate of 5 ℃/min, the temperature is kept for 1 hour under the condition that the temperature is raised to 800 ℃ at the temperature rising rate of 5 ℃/min, and the temperature is kept for 1 hour under the condition that the temperature is raised to 1200 ℃ at the temperature rising rate of 5 ℃/min.
Preferably, the high temperature sintering: in a vacuum sintering furnace, the temperature is kept for 30min at 1750 ℃ and the temperature is kept at 1750 ℃ at the temperature rising rate of 10 ℃/min and the temperature rising rate of 1200 ℃.
Preferably, the annealing: naturally cooling to 500 ℃ in a vacuum sintering furnace, and preserving heat for 30-40min.
The invention also provides a high-purity quartz diffuser which can be mechanically processed to a required shape and is arranged at the top end and the pipe wall of a vent pipe in the CVD chemical vapor deposition equipment.
The invention provides a high-purity quartz diffuser and a preparation method thereof, wherein the method adopts high-purity fumed silica, combines with a deionized water high-speed dispersion process to prepare a high-purity siliceous dispersing agent, and prepares slurry by matching the high-purity siliceous dispersing agent with high-purity nanoscale quartz particles, thereby ensuring the purity of raw materials; after the green body is formed, the multi-temperature section long heat preservation technology is adopted to effectively remove the organic foam and simultaneously prevent the green body from deforming, and the yield of the diffuser prepared by the method provided by the invention can reach more than 80%.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure of the invention as claimed.
Detailed Description
Exemplary embodiments will be described in detail herein. The implementations described in the following exemplary examples do not represent all implementations consistent with the invention. Rather, they are merely examples of systems consistent with aspects of the invention as detailed in the accompanying claims.
The preparation method provided by the embodiment obtains the high-purity quartz diffuser, so that gas can be uniformly diffused in the reaction chamber after passing through the quartz diffuser, and the characteristic can greatly improve the deposition uniformity in the CVD reaction chamber in the wafer preparation process.
The preparation method of the high-purity quartz diffuser in the embodiment comprises the following steps:
step 1: preparing slurry:
high-purity fumed silica and deionized water are dispersed at a high speed to prepare a high-purity siliceous dispersing agent, the content of total metal ions of the high-purity fumed silica is required to be below 50ppm, the conductivity of the deionized water is 16-18MΩ & cm, and the high-purity siliceous dispersing agent is prepared by the following components in parts by weight: 30-40 parts of high-purity fumed silica, 60-70 parts of deionized water, and continuously working for 50-60min at the rotating speed of 1600-1800r/min of a high-speed dispersing machine. The shearing force formed by high rotation speed can recombine the Van der Waals force between molecules to form colloid material mSiO 2 ·nH 2 O·SiO 2 Which is a silica sol without a stabilizer. Then adding quartz micro powder with the purity of more than 99.99999 percent and the granularity of D50200-250nm, and the weight parts are as follows: 35 parts of high-purity siliceous dispersing agent, 65 parts of high-purity quartz micro powder and the rotating speed of a high-speed dispersing machine is 200-300r/min, and the continuous working is carried out for 8-10min.
Step 2: preparing a blank: immersing the pretreated reticulated polyurethane foam into the slurry to fully and uniformly coat the slurry on the polyurethane foam;
specifically, the reticulated polyurethane foam is placed in an ultrasonic cleaning tank, cleaned for 30 seconds, superfluous particles attached to the surface are removed, cleaned by deionized water, placed in an oven, and baked for 30 minutes, wherein the temperature of the oven is 50-55 ℃. The reticular polyurethane foam is immersed into the prepared slurry, the pressure of 5N is applied by using a pp material pressure head to repeatedly squeeze for 8-10 times, the slurry is placed in a centrifuge for 500-600r/min, the continuous working is carried out for 3-4min, and the redundant slurry is thrown away. Placing on pp material filter screen, removing excessive slurry with pure compressed air under 2.5Mpa, and blowing 5-10cm from the surface of the blank body perpendicular to the surface of the blank body for 2-3min to make the slurry fully and uniformly coated on the foam net body. Because the stabilizing agent is not added in the method, redundant slurry can be quickly removed after slurry is thrown away in a centrifugal machine and purged, and the slurry is prevented from coagulating and blocking the pores of polyurethane foam.
Step 3: and (3) blank forming: drying and molding the prepared green body within 120 min;
specifically, in a ventilation drying furnace, ventilation drying is carried out for 60min at the temperature of 100-150 ℃, and pure air is vertical to the lower surface of the blank body and upwards ventilated.
Step 4: volatilizing the organic foam on the surface of the blank after the firing forming;
specifically, in a vacuum sintering furnace, the temperature is kept for 1 hour under the condition that the room temperature is raised to 500 ℃ at the temperature rising rate of 5 ℃/min, the temperature is kept for 1 hour under the condition that the temperature is raised to 800 ℃ at the temperature rising rate of 5 ℃/min, and the temperature is kept for 1 hour under the condition that the temperature is raised to 1200 ℃ at the temperature rising rate of 5 ℃/min.
Step 5: sintering the blank obtained in the step 4 at a high temperature;
specifically, in a vacuum sintering furnace, the temperature is kept for 30min under the conditions of the temperature rising rate of 10 ℃/min and the temperature rising rate of 1200 ℃ to 1750 ℃ and the temperature of 1750 ℃.
Step 6: annealing the sintered blank;
specifically, naturally cooling to 500 ℃ in a vacuum sintering furnace, and preserving heat for 30-40min.
Step 7: and naturally cooling the annealed blank body to room temperature in a vacuum sintering furnace.
In addition, the embodiment also provides a high-purity quartz diffuser, wherein the K+ content of the high-purity quartz diffuser prepared by the method is less than 3.0ppm; na+ content is less than 2.5ppm; compressive strength is 800-1000MPa;50 mm. Times.50 mm sample ventilation: 1.2-1.5L/min;
when the slurry dispersing agent is prepared, the rotating speed of a high-speed dispersing machine is 1600-1800r/min, and the shearing force formed by the high rotating speed can enable the intermolecular van der Waals force to be recombined to form a colloid material mSiO 2 ·nH 2 O·SiO 2 If the rotating speed does not reach the standard, the silicon dioxide particles only suspend in the deionized water and do not form colloid, which affects the subsequent green body preparation, and when the centrifugal machine works, the granular matters of the slurry are separated from the polyurethane foam, so that the uniform coating effect cannot be achieved. Such as the step 1 slurry preparation processThe rotating speed of a high-speed dispersing machine is adjusted to 1400r/min when the high-purity siliceous dispersing agent is prepared, after the high-purity quartz powder is added into slurry, the slurry continuously works for 15min in the high-speed dispersing machine, after extrusion in the step 2, the slurry continuously works for 6min at the rotating speed of 300r/min in a centrifugal machine, and the compression strength of the prepared finished product is 300MPa, and the ventilation volume is only: 0.4L/min. And (3) adjusting the rotating speed of a high-speed dispersing machine when the colloid dispersing agent is prepared in the slurry preparation process in the step (1) to 2000r/min, continuously working in the high-speed dispersing machine for 5min after the slurry is added with high-purity quartz powder, continuously working in a centrifuge for 10min after extrusion in the step (2) at the rotating speed of 300r/min, and obtaining the finished product with the compressive strength of 200MPa and the ventilation volume of only 0.7L/min. The rotational speed of a high-speed dispersing machine when a colloid dispersing agent is prepared in the slurry preparation process in the step 1 is adjusted to 2000r/min, the slurry is continuously operated in the high-speed dispersing machine for 3min after being added with high-purity quartz powder, the slurry is continuously operated in a centrifugal machine for 800r/min in the step 2 for 2min, and the compression strength of a finished product is 500MPa, and the ventilation volume is only: 1.0L/min.
In summary, only by setting reasonable rotation speed and time in the preparation process of the colloid dispersing agent and setting stirring rotation speed and time for adding quartz powder and rotation speed and time for working in a centrifugal machine in combination with the fluidity of the dispersing agent, ideal sintering strength and ventilation capacity can be achieved.
The high-purity quartz diffuser can be machined to a required shape and is arranged at the top end and the pipe wall of a ventilation pipe in the CVD chemical vapor deposition equipment.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
Claims (10)
1. The preparation method of the high-purity quartz diffuser is characterized by comprising the following steps of:
step 1: preparing slurry: according to parts by weight, 30-40 parts of high-purity fumed silica is obtained, 60-70 parts of deionized water are mixed under the condition of high-speed dispersion to obtain a high-purity siliceous dispersing agent, and after standing, 35 parts of the high-purity siliceous dispersing agent and 65 parts of high-purity quartz micro powder are obtained and mixed under the condition of high-speed dispersion to obtain slurry;
step 2: preparing a blank: immersing the pretreated reticulated polyurethane foam into the slurry to fully and uniformly coat the slurry on the polyurethane foam;
step 3: and (3) blank forming: drying and molding the prepared green body within 120 min;
step 4: volatilizing the organic foam on the surface of the blank after the firing forming;
step 5: sintering the blank obtained in the step 4 at a high temperature;
step 6: annealing the sintered blank;
step 7: and naturally cooling the annealed blank body to room temperature in a vacuum sintering furnace.
2. The method for preparing a high purity quartz diffuser according to claim 1, wherein the total metal ion content in the high purity fumed silica is less than 50ppm; the conductivity of the deionized water is 16-18MΩ & cm;
the technological parameters of mixing the high-purity fumed silica and deionized water under the condition of high-speed dispersion are as follows: the rotating speed of the high-speed dispersing machine is 1600-1800r/min, the dispersing time is 120min, and the standing time after mixing is 3-5min;
the purity of the high-purity quartz micro powder is more than 99.99999 percent, and the granularity D 50 200-250nm；
The technological parameters of mixing the high-purity siliceous dispersing agent and the high-purity quartz micro powder under the condition of high-speed dispersion are as follows: the rotating speed of the high-speed dispersing machine is 200-300r/min, and the dispersing time is 30min.
3. The method of preparing a high purity quartz diffuser of claim 1 wherein said slurry is coated on said polyurethane foam comprising the steps of: after the pretreated reticular polyurethane foam is immersed into the slurry, repeatedly extruding the reticular polyurethane foam body for 8-10 times by adopting a PP material pressure head to apply 5N pressure, and then placing the reticular polyurethane foam and the slurry in a centrifuge for 500-600r/min, wherein the treatment time is 3-4min; and taking out the reticular polyurethane foam, placing the reticular polyurethane foam on a pp material filter screen, and removing redundant slurry on the reticular polyurethane foam by adopting pure compressed air.
4. The method for preparing a high purity quartz diffuser according to claim 3, wherein the method for removing redundant slurry on the reticulated polyurethane foam by pure compressed air comprises the following process parameters: the air nozzle is 5-10cm away from the surface of the blank and perpendicular to the surface of the blank for ventilation for 2-3min, and is more than 1cm away from the edge of the net-shaped polyurethane foam of the blank, and the air pressure is 2.5Mpa.
5. A method of preparing a high purity quartz diffuser according to claim 3 wherein the pre-treated reticulated polyurethane foam: placing the reticulated polyurethane foam into an ultrasonic cleaning tank, cleaning for 30s, removing superfluous particles attached to the surface, cleaning with deionized water, placing into an oven, and baking for 30min, wherein the temperature of the oven is 50-55 ℃.
6. The method for preparing a high purity quartz diffuser according to claim 1, wherein the drying and molding the prepared green body comprises: and (3) in a ventilation drying furnace, ventilating and drying for 60 minutes at the temperature of 100-150 ℃, and ventilating pure air upwards perpendicular to the lower surface of the blank.
7. The method for preparing a high purity quartz diffuser according to claim 1, wherein the temperature-increasing procedure of the volatilized and burned organic foam is as follows: in a vacuum sintering furnace, the temperature is kept for 1 hour under the condition that the room temperature is raised to 500 ℃ at the temperature rising rate of 5 ℃/min, the temperature is kept for 1 hour under the condition that the temperature is raised to 800 ℃ at the temperature rising rate of 5 ℃/min, and the temperature is kept for 1 hour under the condition that the temperature is raised to 1200 ℃ at the temperature rising rate of 5 ℃/min.
8. The method for preparing a high purity quartz diffuser according to claim 1, wherein the high temperature sintering: in a vacuum sintering furnace, the temperature is kept for 30min at 1750 ℃ and the temperature is kept at 1750 ℃ at the temperature rising rate of 10 ℃/min and the temperature rising rate of 1200 ℃.
9. The method for preparing a high purity quartz diffuser according to claim 1, wherein the annealing: naturally cooling to 500 ℃ in a vacuum sintering furnace, and preserving heat for 30-40min.
10. A high purity quartz diffuser produced by the method of claims 1-9, wherein the high purity quartz diffuser is mechanically machined to a desired shape and is mounted to the top and walls of a vent tube in a CVD chemical vapor deposition apparatus.
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