CN114029300A - Method for cleaning graphite plate - Google Patents
Method for cleaning graphite plate Download PDFInfo
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- CN114029300A CN114029300A CN202110271196.8A CN202110271196A CN114029300A CN 114029300 A CN114029300 A CN 114029300A CN 202110271196 A CN202110271196 A CN 202110271196A CN 114029300 A CN114029300 A CN 114029300A
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- cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
- B08B9/20—Cleaning containers, e.g. tanks by using apparatus into or on to which containers, e.g. bottles, jars, cans are brought
- B08B9/22—Cleaning containers, e.g. tanks by using apparatus into or on to which containers, e.g. bottles, jars, cans are brought the apparatus cleaning by soaking alone
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/14—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects using gases or vapours other than air or steam, e.g. inert gases
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/22—Controlling the drying process in dependence on liquid content of solid materials or objects
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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Abstract
The invention relates to a method for cleaning a graphite disc, which comprises the following steps: cleaning a graphite disc for the first time by using a first cleaning solution, wherein the first cleaning solution is an alkaline cleaning solution; cleaning the graphite disc for the second time by using a second cleaning solution, wherein the second cleaning solution is an alkaline cleaning solution added with an oxidant; cleaning the graphite disc for the third time by using a third cleaning solution, wherein the third cleaning solution is an acid cleaning solution; cleaning the graphite disc for the fourth time by using a fourth cleaning solution, wherein the fourth cleaning solution is deionized water; and drying the graphite disc to obtain the graphite disc with the required specification. The cleaning method is simple to operate, low in cost and good in cleaning effect, high-temperature baking and cleaning in an MOCVD furnace are not needed, and the problems existing in the conventional graphite plate cleaning mode can be solved.
Description
Technical Field
The invention relates to the technical field of semiconductor manufacturing, in particular to a method for cleaning a graphite disc.
Background
Arsenic-phosphorus (As/P) series compound semiconductor materials have been widely used in the fields of red and yellow Light Emitting Diodes (LEDs), solar cells, and the like, and most of them use a Metal-organic Chemical Vapor Deposition (MOCVD) growth method to heat a graphite plate by a heating device. Specifically, arsenic-phosphorus series compounds are used as growth source materials and placed on a graphite plate, and epitaxial structures such as LEDs and solar cells are grown on a substrate in a thermal decomposition reaction mode. After the graphite plate is used for a certain number of times, certain arsenic and phosphorus impurities can be deposited on the surface of the graphite plate, and if the arsenic and phosphorus impurities on the graphite plate are not cleaned in time, the epitaxial growth quality of the graphite plate can be influenced.
At present, the common graphite plate cleaning mode is as follows: high-temperature baking in an oven-outside baking tray furnace or an MOCVD furnace. However, although a plurality of graphite plates can be baked at a time by the baking of the baking pan outside the oven at a high temperature, the energy consumption cost is high, and if only a small number of graphite plates are baked by the baking pan, the baking cost of a single graphite plate is too high; the high temperature in the MOCVD furnace is high, and the long-time high temperature can damage the existing stable chamber environment of the reaction chamber.
Disclosure of Invention
In view of the defects of the prior art, an object of the present application is to provide a method for cleaning a graphite plate, which is not only simple in operation, low in cost and good in cleaning effect, but also does not need to use a high-temperature baking cleaning in an MOCVD furnace, and aims to solve the problems that the cleaning cost of the graphite plate cleaning method is high and the temperature in the furnace required by the high-temperature baking cleaning is high in the prior art.
A method of cleaning a graphite disk, comprising: cleaning a graphite disc for the first time by using a first cleaning solution, wherein the first cleaning solution is an alkaline cleaning solution; cleaning the graphite disc for the second time by using a second cleaning solution, wherein the second cleaning solution is an alkaline cleaning solution added with an oxidant; cleaning the graphite disc for the third time by using a third cleaning solution, wherein the third cleaning solution is an acid cleaning solution; cleaning the graphite disc for the fourth time by using a fourth cleaning solution, wherein the fourth cleaning solution is deionized water; and drying the graphite disc to obtain the graphite disc with the required specification.
The cleaning method of the graphite plate is simple to operate, low in cost and good in cleaning effect, high-temperature baking and cleaning in an MOCVD furnace are not needed, and the problems existing in the conventional graphite plate cleaning mode can be solved.
Optionally, the first cleaning of the graphite disc with the first cleaning solution includes: sealing the graphite disc; placing the sealed graphite disc on a cleaning frame; putting the graphite disc into the first cleaning solution for soaking; carrying out first bubbling cleaning on the soaked graphite disc; brushing the surface of the graphite disc cleaned by the first bubbling; and carrying out secondary bubbling cleaning on the graphite disk.
Optionally, the second cleaning of the graphite disc with a second cleaning solution includes: carrying out third bubbling cleaning on the graphite disc; brushing the surface of the graphite disc cleaned by the third bubbling; and carrying out fourth bubbling cleaning on the graphite disc.
Optionally, the third cleaning of the graphite disc with a third cleaning solution includes: carrying out first deionized water washing on the graphite disc; and putting the graphite disc into the third cleaning solution for fifth bubbling cleaning.
Optionally, the fourth cleaning of the graphite disc with a fourth cleaning solution includes: carrying out secondary deionized water washing on the graphite disc; putting the graphite disc into the fourth cleaning solution for carrying out sixth bubbling cleaning; carrying out third deionized water washing on the graphite disc; putting the graphite disc into the fourth cleaning solution for carrying out seventh bubbling cleaning; and carrying out deionized water washing on the graphite disc for the fourth time.
Optionally, the drying the graphite disc to obtain a graphite disc with a required specification includes: removing moisture on the surface of the graphite disc; baking the graphite disc for the first time; baking the graphite disc for the second time; and blowing the surface of the graphite disc to obtain the graphite disc with the required specification.
Alternatively, the time for the first bubble cleaning is 30 minutes, the time for the second bubble cleaning is 10 to 20 minutes, the time for the third bubble cleaning is 60 minutes, the time for the fourth bubble cleaning is 60 minutes, the time for the fifth bubble cleaning is 60 minutes, the time for the sixth bubble cleaning is 20 to 40 minutes, and the time for the seventh bubble cleaning is 60 minutes.
Optionally, the bubble pressures of the first bubble cleaning, the second bubble cleaning, the third bubble cleaning, the fourth bubble cleaning, the fifth bubble cleaning, the sixth bubble cleaning and the seventh bubble cleaning are all 0.1 to 0.3 MPa.
Optionally, the temperature of the first baking is 100 ℃, and the baking time of the first baking is 1-2 hours; the temperature of the second baking is 200 ℃, and the baking time of the second baking is 4-6 hours.
Optionally, the first cleaning solution is ammonia water with a concentration of 20-30%, the second cleaning solution is a mixed solution prepared from 2 parts of ammonia water with a concentration of 20-30% and 1 part of hydrogen peroxide with a concentration of 20-30%, and the third cleaning solution is hydrogen fluoride solution with a concentration of 15-20%.
In conclusion, the cleaning method of the graphite plate mainly adopts a chemical solution mode, and can better remove arsenic-phosphorus compounds on the graphite plate of the arsenic-phosphorus series MOCVD equipment. Moreover, the method for cleaning the graphite plate is simple to operate, low in cost and good in cleaning effect, and does not need to use high-temperature baking and cleaning outside a large-scale high-temperature baking plate furnace or in an MOCVD furnace. Therefore, the cleaning method of the graphite plate solves the problems that the cleaning cost of the cleaning mode in the prior art is high and the temperature in the furnace required by high-temperature baking and cleaning is high.
Drawings
Fig. 1 is a schematic flow chart of a method for cleaning a graphite disc disclosed in an embodiment of the present application;
FIG. 2 is a schematic flow chart illustrating the sub-step of step S50 in the cleaning method shown in FIG. 1;
FIG. 3 is a schematic flow chart illustrating the sub-step of step S20 in the cleaning method shown in FIG. 1;
FIG. 4 is a schematic flow chart illustrating the sub-step of step S30 in the cleaning method shown in FIG. 1;
FIG. 5 is a schematic flow chart illustrating the sub-step of step S40 in the cleaning method shown in FIG. 1;
fig. 6 is a flowchart illustrating a sub-step of step S50 in the cleaning method shown in fig. 1.
Description of reference numerals:
S10-S50-step of the method for cleaning graphite plate;
S11-S16-substep of step S10;
S21-S23-substep of step S20;
S31-S32-substep of step S30;
S41-S45-substep of step S40;
S51-S54-substep of step S50.
Detailed Description
To facilitate an understanding of the present application, the present application will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present application are given in the accompanying drawings. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application.
Nowadays, arsenic-phosphorus (As/P) series compound semiconductor materials are widely used in the fields of red-yellow light LEDs, solar cells and the like, and most of the materials adopt the MOCVD growth mode, and a graphite plate is heated by a heating device. Specifically, arsenic-phosphorus series compounds are used as growth source materials and placed on a graphite plate, and epitaxial structures such as LEDs and solar cells are grown on a substrate in a thermal decomposition reaction mode. However, after the graphite plate is used for a certain number of times, certain arsenic and phosphorus impurities are deposited on the surface of the graphite plate, and if the arsenic and phosphorus impurities on the graphite plate are not cleaned in time, the epitaxial growth quality of the graphite plate is affected. At present, the common graphite plate cleaning mode is as follows: high-temperature baking in an oven-outside baking tray furnace or an MOCVD furnace. However, although a plurality of graphite plates can be baked at a time by the baking of the baking pan outside the oven at a high temperature, the energy consumption cost is high, and if only a small number of graphite plates are baked by the baking pan, the baking cost of a single graphite plate is too high; the high temperature in the MOCVD furnace is high, and the long-time high temperature may damage a stable chamber environment of the reaction chamber or needs a plurality of furnaces to grow and then can be recovered to a good chamber environment for epitaxial growth. Therefore, how to solve the problems that the cleaning cost of the graphite plate cleaning mode is high and the temperature in the furnace required by high-temperature baking cleaning is high in the prior art is a critical need to be solved.
Based on this, the present application hopes to provide a solution to the above technical problems, which is not only simple in operation, low in cost, and better in cleaning effect, but also does not need to use the high temperature baking cleaning in the MOCVD furnace, and can improve the problems existing in the existing graphite plate cleaning manner, and the details thereof will be explained in the following embodiments.
The scheme of the application elaborates the cleaning method of the graphite disc.
Please refer to fig. 1, which is a schematic flow chart illustrating a method for cleaning a graphite plate according to an embodiment of the present application. In the embodiment of the application, the graphite plate is used for an arsenic-phosphorus series MOCVD device, the cleaning method of the graphite plate mainly adopts a chemical solution mode to clean the graphite plate, and the whole cleaning method is simple in operation, low in cost and good in cleaning effect, and does not need to use high-temperature baking and cleaning outside a large-scale high-temperature baking plate furnace or in an MOCVD furnace. In this embodiment, as shown in fig. 1, the method for cleaning the graphite disc at least includes the following steps.
And step S10, carrying out first cleaning on the graphite disc by using a first cleaning solution.
Specifically, referring to fig. 2, in the embodiment of the present application, the "performing a first cleaning on a graphite disc with a first cleaning solution" includes at least the following steps.
And step S11, sealing the graphite disc.
Specifically, in the present embodiment, the graphite plate may be wrapped with an aluminum foil, and the wrapped graphite plate may be placed in a sealed bag (e.g., a Polyvinyl chloride (PVC) bag) to seal the graphite plate.
And step S12, placing the sealed graphite disc on a cleaning frame.
Specifically, in the embodiment of the application, the graphite plate wrapped in the sealed bag is moved to a cleaning frame so as to facilitate subsequent operation. Wherein, the cleaning frame can be a cleaning groove frame used for fixing the graphite plate.
And step S13, putting the graphite disc into the first cleaning solution for soaking.
Specifically, in this application embodiment, after will seal the graphite dish is placed on the wash rack after, open the cleaning machine and exhaust, will the sealed package of graphite dish is unpack apart, then will the graphite dish is put into in the first cleaning solution, close after putting the protection window of cleaning machine, and soak a predetermined soaking time in the first cleaning solution.
In the embodiment of the present application, the first cleaning solution may be an alkaline cleaning solution, for example: ammonia water of 20-30% concentration, for example: 20% ammonia, 22% ammonia, 25% ammonia, 27% ammonia, 28% ammonia, or other concentrations of ammonia. The preset soaking time is 60 minutes, impurities such as arsenic and phosphorus compounds on the surface of the graphite disc can be well cleaned through soaking operation in the first cleaning solution, and the function of the cleaning solution is mainly an acid-base neutralization principle. In this step, since the surface of the graphite plate has more arsenic-phosphorus compounds, it is not preferable to accelerate the process by bubbling cleaning.
And step S14, carrying out first bubbling cleaning on the soaked graphite disc.
Specifically, in the embodiment of the present application, after the graphite plate is placed in the first cleaning solution and soaked for the predetermined soaking time, nitrogen gas is introduced into the first cleaning solution to perform first bubbling cleaning, and the time for the first bubbling cleaning is 30 minutes.
In an embodiment of the present application, the bubbling pressure of the first bubbling cleaning is 0.1 to 0.3MPa, and for example: 0.1MPa, 0.15MPa, 0.2MPa, 0.25MPa, or other values.
And step S15, brushing the surface of the graphite disc cleaned by the first bubbling.
Specifically, in the embodiment of the present invention, after the first bubbling cleaning of the graphite plate, the surface of the graphite plate is brushed in a reciprocating manner, and for example, the surface of the graphite plate may be brushed in a reciprocating manner by a brushing tool such as a plastic brush. Based on the reciprocating rinsing operation, impurities such as the arsenic-phosphorus compound layer and the like which are not completely fallen off after the surface of the graphite plate is cleaned by the first cleaning solution can be removed, most of the impurities such as the arsenic-phosphorus compound layer and the like which are not completely fallen off can be brushed off after the reciprocating brushing operation, and the arsenic-phosphorus compound layer which is not cleaned can be exposed.
And step S16, carrying out secondary bubbling cleaning on the graphite disc.
Specifically, in the embodiment of the present application, after the surface of the graphite plate is brushed, nitrogen gas is introduced into the first cleaning solution to perform the second bubbling cleaning, and the time for the second bubbling cleaning is 10 to 20 minutes, for example: 10 minutes, 12 minutes, 15 minutes, 17 minutes, 19 minutes, or other values.
In an embodiment of the present application, the bubbling pressure of the second bubbling cleaning is 0.1 to 0.3MPa, and for example: 0.1MPa, 0.15MPa, 0.2MPa, 0.25MPa, or other values.
In this step, the graphite plate after being soaked is subjected to first bubbling cleaning and second bubbling cleaning, so that the first cleaning solution in the cleaning machine flows, the reaction between the first cleaning solution and the arsenic-phosphorus compound on the surface of the graphite plate is accelerated, and the arsenic-phosphorus compound on the surface of the graphite plate can be removed, that is, the first bubbling cleaning and the second bubbling cleaning mainly accelerate the reaction between the first cleaning solution and the arsenic-phosphorus compound on the surface of the graphite plate, thereby achieving the effect of accelerating cleaning.
And step S20, carrying out secondary cleaning on the graphite disc by using a second cleaning solution.
Specifically, in the embodiment of the present application, after the first bubbling cleaning and the second bubbling cleaning are performed on the graphite disk, the cleaning solution is replaced, and the second cleaning operation is performed on the graphite disk using the second cleaning solution.
In the embodiment of the present application, the second cleaning solution may be an alkaline cleaning solution added with an oxidizing agent, for example: the mixed solution prepared from 2 parts of ammonia water with the concentration of 20-30% and 1 part of hydrogen peroxide with the concentration of 20-30% is also the mixed solution with the ratio of the ammonia water to the hydrogen peroxide of 2:1, and is, for example: 20% ammonia, 22% ammonia, 25% ammonia, 27% ammonia, 28% ammonia, or other concentrations of ammonia. The concentration of the hydrogen peroxide in the second cleaning solution can be, for example: 20% hydrogen peroxide, 22% hydrogen peroxide, 25% hydrogen peroxide, 27% hydrogen peroxide, 28% hydrogen peroxide, or other concentrations of hydrogen peroxide.
Specifically, referring to fig. 3, in the embodiment of the present application, the "performing the second cleaning on the graphite disc with the second cleaning solution" includes at least the following steps.
And step S21, carrying out third bubbling cleaning on the graphite disc.
Specifically, in the embodiment of the present application, after the graphite plate is placed in the second cleaning solution, nitrogen gas is introduced into the second cleaning solution to perform the third bubbling cleaning, and the time for the third bubbling cleaning is 60 minutes. In the step, most arsenic and phosphorus compounds on the surface of the graphite plate are not generated, and the hydrogen peroxide is added into the ammonia water and then the bubbling cleaning operation is carried out, so that the reaction is not too violent, and the aim of accelerating the reaction is fulfilled on the premise of ensuring the safe cleaning operation.
In an embodiment of the present application, the bubble pressure of the third bubble cleaning is 0.1 to 0.3MPa, for example: 0.1MPa, 0.15MPa, 0.2MPa, 0.25MPa, or other values.
And step S22, brushing the surface of the graphite disc cleaned by the third bubbling.
Specifically, in the embodiment of the present invention, after the graphite plate is subjected to the third bubbling cleaning, the surface of the graphite plate is brushed in a reciprocating manner, for example, the surface of the graphite plate may be brushed in a reciprocating manner by a brushing tool such as a plastic brush. Based on the reciprocating rinsing operation, impurities such as the arsenic-phosphorus compound layer and the like which are not completely fallen off after the surface of the graphite plate is cleaned by the second cleaning solution can be removed, most of the impurities such as the arsenic-phosphorus compound layer and the like which are not completely fallen off can be brushed off after the graphite plate is repeatedly brushed, and the arsenic-phosphorus compound layer which is not cleaned can be exposed.
And step S23, carrying out bubbling cleaning on the graphite disc for the fourth time.
Specifically, in the embodiment of the present application, after the surface of the graphite disk is brushed, nitrogen gas is introduced into the second cleaning solution to perform the fourth bubbling cleaning, and the time for the fourth bubbling cleaning is 60 minutes. In the step, most arsenic and phosphorus compounds on the surface of the graphite plate are not generated, and the hydrogen peroxide is added into the ammonia water and then the bubbling cleaning operation is carried out, so that the reaction is not too violent, and the aim of accelerating the reaction is fulfilled on the premise of ensuring the safe cleaning operation.
In the present embodiment, the bubbling pressure in the fourth bubbling cleaning is also 0.1 to 0.3MPa, and is, for example: 0.1MPa, 0.15MPa, 0.2MPa, 0.25MPa, or other values.
And step S30, carrying out third cleaning on the graphite disc by using a third cleaning solution.
Specifically, in the embodiment of the present invention, after the graphite plate is subjected to the fourth bubbling cleaning, the cleaning solution is replaced, and the third cleaning operation is performed on the graphite plate using the third cleaning solution.
In an embodiment of the present application, the third cleaning solution may be an acidic cleaning solution, such as: 15-20% hydrogen fluoride (formula HF) solution, again for example: hydrogen fluoride at 15% concentration, hydrogen fluoride at 17% concentration, hydrogen fluoride at 18% concentration, hydrogen fluoride at 19% concentration, or other concentrations.
Specifically, referring to fig. 4, in the embodiment of the present application, the "performing a third cleaning on the graphite disc with a third cleaning solution" includes at least the following steps.
And step S31, washing the graphite disc with Deionized water (Deionized water) for the first time.
Specifically, in this application embodiment, the graphite tray is taken out after nitrogen gas is introduced into the second cleaning solution to perform bubbling cleaning for the fourth time, and the graphite tray is subjected to deionized water washing operation for the first time, for example, the deionized water gun can be used for washing operation, so that the effect of cleaning the second cleaning solution remaining on the surface of the graphite tray can be achieved.
And step S32, placing the graphite disc into the third cleaning solution for fifth bubbling cleaning.
Specifically, in the embodiment of the present application, after the first deionized water rinsing operation is performed on the graphite disc, the graphite disc is placed in the third cleaning solution to perform a fifth bubbling cleaning, and the time for the fifth bubbling cleaning is 60 minutes. By performing the fifth bubbling cleaning operation in the third cleaning solution, impurities such as arsenic and phosphorus compounds that have not been removed from the surface of the graphite disk can be further removed.
In the present embodiment, the bubbling pressure of the fifth bubbling cleaning is also 0.1 to 0.3MPa, and for example: 0.1MPa, 0.15MPa, 0.2MPa, 0.25MPa, or other values.
And step S40, cleaning the graphite disc for the fourth time by using a fourth cleaning solution.
Specifically, in the embodiment of the present application, after the graphite plate is placed in the third cleaning solution and subjected to the fifth bubbling cleaning, the graphite plate is subjected to the fourth cleaning operation, so that the chemical solution remaining on the surface of the graphite plate can be cleaned, and preparation is made for the subsequent use of the graphite plate.
In an embodiment of the present application, the fourth cleaning solution is deionized water.
Specifically, referring to fig. 5, in the embodiment of the present application, the "performing a fourth cleaning on the graphite disc with a fourth cleaning solution" includes at least the following steps.
And step S41, carrying out secondary deionized water washing on the graphite disc.
Specifically, in the embodiment of the present application, after the graphite disc is subjected to the fifth bubbling cleaning in the third cleaning solution, the graphite disc is taken out, and the graphite disc is subjected to the second deionized water washing operation, for example, the deionized water gun can be used for washing, so that the effect of cleaning the chemical solution remaining on the surface of the graphite disc can be achieved.
And step S42, putting the graphite disc into the fourth cleaning solution for sixth bubbling cleaning.
Specifically, in the embodiment of the present application, after the graphite disc is subjected to the second deionized water rinsing operation, the graphite disc is put into the fourth cleaning solution to be subjected to sixth bubble cleaning, and the time for the sixth bubble cleaning is 20 to 40 minutes, and may be, for example: 20 minutes, 25 minutes, 30 minutes, 34 minutes, 36 minutes, 38 minutes, or other values. In this step, the graphite plate is subjected to a sixth bubbling cleaning operation in the fourth cleaning solution, so that an effect of cleaning the chemical solution remaining on the surface of the graphite plate is achieved.
In an embodiment of the present application, the bubble pressure of the sixth bubble cleaning is 0.1 to 0.3MPa, and for example: 0.1MPa, 0.15MPa, 0.2MPa, 0.25MPa, or other values.
And step S43, carrying out third deionized water washing on the graphite disc.
Specifically, in the embodiment of the present application, after the graphite disc is subjected to the sixth bubbling cleaning in the fourth cleaning solution, the graphite disc is taken out, and the graphite disc is subjected to a third deionized water washing operation, for example, a deionized water gun can be used for washing, so that the chemical solution remaining on the surface of the graphite disc can be further cleaned.
And step S44, placing the graphite disc into the fourth cleaning solution for carrying out seventh bubbling cleaning.
Specifically, in the embodiment of the present application, after the graphite disc is subjected to the third deionized water rinsing operation, the graphite disc is put into a fresh fourth cleaning solution to be subjected to the seventh bubbling cleaning, and the time for the seventh bubbling cleaning is 60 minutes. In this step, the graphite plate may be further cleaned with a chemical solution remaining on the surface of the graphite plate by performing a seventh bubbling cleaning operation in the fourth cleaning solution.
In an embodiment of the present application, the bubble pressure of the seventh bubble cleaning is 0.1 to 0.3MPa, and for example: 0.1MPa, 0.15MPa, 0.2MPa, 0.25MPa, or other values.
And step S45, performing deionized water washing on the graphite disc for the fourth time.
Specifically, in the embodiment of the present application, after the graphite plate is subjected to the seventh bubbling cleaning in the fourth cleaning solution, the graphite plate is taken out, and the graphite plate is subjected to the fourth deionized water washing operation, for example, the deionized water gun can be used for washing, so that the chemical solution remaining on the surface of the graphite plate can be further cleaned.
And step S50, drying the graphite disc to obtain the graphite disc with the required specification.
Specifically, in the embodiment of the present application, after the graphite disc is placed in the fourth cleaning solution to be cleaned for the fourth time, the residual chemical solution on the surface of the graphite disc is cleaned, and at this time, moisture on the surface of the graphite disc needs to be removed, so as to obtain the graphite disc meeting the specifications of required cleanliness, dryness and the like, and further, the graphite disc can be used in an arsenic-phosphorus series MOCVD apparatus.
Specifically, referring to fig. 6, in the embodiment of the present application, the step of "drying the graphite disc to obtain a graphite disc with a desired specification" includes at least the following steps.
And step S51, removing moisture on the surface of the graphite disc.
Specifically, in the embodiment of the present invention, after the graphite plate is subjected to the fourth deionized water rinsing operation, the moisture on the surface of the graphite plate is removed, and the moisture on the surface of the graphite plate may be dried by, for example, a nitrogen gun.
And step S52, baking the graphite disc for the first time.
Specifically, in the embodiment of the present application, after removing moisture on the surface of the graphite plate, the graphite plate is placed in an oven for a first baking operation, which mainly serves to remove moisture on the surface of the graphite plate. In this embodiment, the first baking temperature may be 100 degrees, and the baking time of the first baking may be 1-2 hours, for example, 1 hour, 1.2 hours, 1.5 hours, 1.8 hours, or other values.
And step S53, baking the graphite disc for the second time.
Specifically, in this application embodiment, will after the graphite plate was put into the oven and is carried out the operation of toasting for the first time, it is right to continue the graphite plate carries out the operation of toasting for the second time, and its effect is mainly used for with the surperficial steam of graphite plate toasts completely, reaches the effect of no steam.
In this embodiment, the temperature of the second baking may be 200 degrees, and the baking time of the second baking may be 4 to 6 hours, for example, 4 hours, 4.5 hours, 5 hours, 5.2 hours, 5.5 hours, or other values.
And step S54, purging the surface of the graphite disc to obtain the graphite disc with the required specification.
Specifically, in the embodiment of the present application, after the graphite plate is baked for the second time, the graphite plate is taken out, and impurities possibly present on the surface of the graphite plate are purged, for example, impurities possibly adhered to the surface of the graphite plate may be purged by a nitrogen gun, so that the graphite plate meeting the requirements of cleanliness, dryness and the like is obtained, and further, the graphite plate can be used in an arsenic-phosphorus series MOCVD apparatus.
In conclusion, the cleaning method of the graphite plate mainly adopts a chemical solution mode, and can better remove arsenic-phosphorus compounds on the graphite plate of the arsenic-phosphorus series MOCVD equipment. Moreover, the method for cleaning the graphite plate is simple to operate, low in cost and good in cleaning effect, and does not need to use high-temperature baking and cleaning outside a large-scale high-temperature baking plate furnace or in an MOCVD furnace. Therefore, the cleaning method of the graphite plate solves the problems that the cleaning cost of the cleaning mode in the prior art is high and the temperature in the furnace required by high-temperature baking and cleaning is high.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for cleaning a graphite disc is characterized by comprising the following steps:
cleaning a graphite disc for the first time by using a first cleaning solution, wherein the first cleaning solution is an alkaline cleaning solution;
cleaning the graphite disc for the second time by using a second cleaning solution, wherein the second cleaning solution is an alkaline cleaning solution added with an oxidant;
cleaning the graphite disc for the third time by using a third cleaning solution, wherein the third cleaning solution is an acid cleaning solution;
cleaning the graphite disc for the fourth time by using a fourth cleaning solution, wherein the fourth cleaning solution is deionized water;
and drying the graphite disc to obtain the graphite disc with the required specification.
2. The cleaning method of claim 1, wherein the first cleaning of the graphite disk with the first cleaning solution comprises:
sealing the graphite disc;
placing the sealed graphite disc on a cleaning frame;
putting the graphite disc into the first cleaning solution for soaking;
carrying out first bubbling cleaning on the soaked graphite disc;
brushing the surface of the graphite disc cleaned by the first bubbling;
and carrying out secondary bubbling cleaning on the graphite disk.
3. The method of cleaning of claim 2, wherein the second cleaning of the graphite disk with the second cleaning solution comprises:
carrying out third bubbling cleaning on the graphite disc;
brushing the surface of the graphite disc cleaned by the third bubbling;
and carrying out fourth bubbling cleaning on the graphite disc.
4. The method of cleaning according to claim 3, wherein the third cleaning of the graphite disk with a third cleaning solution comprises:
carrying out first deionized water washing on the graphite disc;
and putting the graphite disc into the third cleaning solution for fifth bubbling cleaning.
5. The method of cleaning according to claim 4, wherein the fourth cleaning of the graphite disk with the fourth cleaning solution comprises:
carrying out secondary deionized water washing on the graphite disc;
putting the graphite disc into the fourth cleaning solution for carrying out sixth bubbling cleaning;
carrying out third deionized water washing on the graphite disc;
putting the graphite disc into the fourth cleaning solution for carrying out seventh bubbling cleaning;
and carrying out deionized water washing on the graphite disc for the fourth time.
6. The method of cleaning according to claim 5, wherein said drying the graphite disk to obtain a desired size graphite disk comprises:
removing moisture on the surface of the graphite disc;
baking the graphite disc for the first time;
baking the graphite disc for the second time;
and blowing the surface of the graphite disc to obtain the graphite disc with the required specification.
7. The cleaning method according to claim 5, wherein the time for the first bubble cleaning is 30 minutes, the time for the second bubble cleaning is 10 to 20 minutes, the time for the third bubble cleaning is 60 minutes, the time for the fourth bubble cleaning is 60 minutes, the time for the fifth bubble cleaning is 60 minutes, the time for the sixth bubble cleaning is 20 to 40 minutes, and the time for the seventh bubble cleaning is 60 minutes.
8. The cleaning method according to claim 5, wherein the bubble gas pressure of each of the first bubble cleaning, the second bubble cleaning, the third bubble cleaning, the fourth bubble cleaning, the fifth bubble cleaning, the sixth bubble cleaning, and the seventh bubble cleaning is 0.1 to 0.3 MPa.
9. The cleaning method according to claim 6, wherein the temperature of the first baking is 100 degrees, and the baking time of the first baking is 1 to 2 hours; the temperature of the second baking is 200 ℃, and the baking time of the second baking is 4-6 hours.
10. The cleaning method according to any one of claims 1 to 9, wherein the first cleaning solution is an ammonia water having a concentration of 20 to 30%, the second cleaning solution is a mixed solution prepared from 2 parts of an ammonia water having a concentration of 20 to 30% and 1 part of a hydrogen peroxide solution having a concentration of 20 to 30%, and the third cleaning solution is a hydrogen fluoride solution having a concentration of 15 to 20%.
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