CN114669546A - Method for cleaning indium phosphide polycrystal material - Google Patents
Method for cleaning indium phosphide polycrystal material Download PDFInfo
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- CN114669546A CN114669546A CN202210403210.XA CN202210403210A CN114669546A CN 114669546 A CN114669546 A CN 114669546A CN 202210403210 A CN202210403210 A CN 202210403210A CN 114669546 A CN114669546 A CN 114669546A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/02—Cleaning by the force of jets or sprays
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/102—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
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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
Abstract
The invention provides a method for cleaning an indium phosphide polycrystal material, which comprises the following steps: and sequentially immersing the indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then performing ultrasonic cleaning in water, and finally dehydrating and drying to finish cleaning. According to the invention, the bromomethanol is used for corroding and cleaning gaps and holes which cannot be polished by some abrasive paper, so that the subsequent cleaning steps are facilitated; second step, cleaning with HF acid to remove SiO on the surface of the crystal bar2And (5) cleaning. The third step is to wash with HCl and to form SiO on the surface2After being cleaned, HCl can quickly react with other impurity elements to clean other impurities in a short time, which is 15 hours and long in cleaning time compared with the original cleaning processGreatly shortened and improved work efficiency.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to a method for cleaning an indium phosphide polycrystal material.
Background
Indium phosphide is a group III-V compound semiconductor formed by combining a group IIIA element indium In and a group VA element P. With the gradual development of application requirements of photoelectrons, microelectronic devices and the like, the superior performance of indium phosphide materials is gradually highlighted, particularly in the field of optical fiber communication, only the indium phosphide semiconductor technology can integrate a photodetector and a laser with other analog and mixed signal functions on the same substrate, and the indium phosphide substrate has the advantages of high integration level and low price, so that the optical devices realize major breakthrough; in the wireless field, indium phosphide amplifiers have been greatly improved in many ways, including improved performance and reduced power consumption; in the millimeter wave application aspect which can not be achieved by other semiconductor materials such as indium arsenide, silicon and the like, passive imaging and other some latest applications can be easily achieved through the indium phosphide device.
A large amount of indium phosphide polycrystal materials are required to be added in the production process of the indium phosphide single crystal, the indium phosphide polycrystal materials are inevitably collided in the growth and processing processes, surface pits and cracks are caused, the surface is oxidized or some grease and metal impurities are introduced, serious influence is caused on the growth of the indium phosphide single crystal, the yield is low, and the cost is high. Therefore, the method for cleaning the indium phosphide polycrystal material is particularly important for improving the yield of the indium phosphide single crystal and reducing the cost.
The existing indium phosphide polycrystal material cleaning process generally uses a mixed solution of ammonia water, hydrogen peroxide and water for cleaning, so that the cleaning time is long, the efficiency is low, only some crystal bars with smooth and flat surfaces can be cleaned, some crystal bars with holes and cracks cannot be treated or cannot be cleaned completely, more impurity elements are remained in gaps after cleaning, and the yield of indium phosphide single crystals is seriously influenced.
Therefore, a new method for cleaning an indium phosphide polycrystal material is needed to solve the current problems, improve the yield of an indium phosphide single crystal and reduce the cost.
Disclosure of Invention
The invention aims to provide a method for cleaning an indium phosphide polycrystal material, which solves the problems of unclean cleaning and low cleaning efficiency of the existing process, improves the yield of indium phosphide single crystals, reduces the production cost and improves the market competitiveness.
The invention provides a method for cleaning an indium phosphide polycrystal material, which comprises the following steps:
sequentially immersing the indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then performing ultrasonic cleaning in water, and finally dehydrating and drying to finish cleaning;
the volume concentration of the bromomethanol is 2-5%, and the cleaning time is 30-60 s; the concentration of the hydrofluoric acid solution is 0.5-2 mol/L, and the cleaning time is 30-60 min; the concentration of the hydrochloric acid solution is 2-4 mol/L, and the cleaning time is 10-30 min.
Preferably, the indium phosphide polycrystal material is washed by deionized water for 2-5 times respectively after being washed by bromomethanol, hydrofluoric acid solution and hydrochloric acid solution.
Preferably, the frequency of the ultrasound is 30-50 Hz.
Preferably, 3-5 times of ultrasonic cleaning are carried out, and the time of each ultrasonic cleaning is 30-60 min.
Preferably, the temperature of the ultrasonic cleaning is 40-70 ℃.
Preferably, the dehydration is performed by soaking the indium phosphide polycrystal material in absolute ethyl alcohol for 2-5 min.
Preferably, the bromomethanol, hydrofluoric acid solution and hydrochloric acid solution cleaning is performed under stirring.
Preferably, the drying is carried out by blow-drying with high-purity nitrogen and then drying.
The invention provides a method for cleaning an indium phosphide polycrystal material, which comprises the following steps: sequentially immersing the indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then performing ultrasonic cleaning in water, and finally dehydrating and drying to finish cleaning; the volume concentration of the bromomethanol is 2-5%, and the cleaning time is 30-60 s; the concentration of the hydrofluoric acid solution is 0.5-2 mol/L, and the cleaning time is 30-60 min; the concentration of the hydrochloric acid solution is 2-4 mol/L, and the cleaning time is 10-30 min. According to the invention, the bromomethanol is used for corroding and cleaning gaps and holes which cannot be polished by some abrasive paper, so that the subsequent cleaning steps are facilitated; the second step is to clean with HF acid, the InP polycrystal material contacts the quartz piece for a long time in the growth process, and the Si element is generally SiO2Shape ofThe SiO on the outer surface of the crystal bar is firstly treated by HF acid to tightly cover the outer surface of the crystal bar and influence the cleaning of other impurities2And (5) cleaning. The third step is to wash with HCl and to make SiO on the surface2After the cleaning, HCl can rapidly react with other impurity elements, so that other impurities can be cleaned in a short time, the cleaning time is greatly shortened compared with 15 hours in the original cleaning process, and the working efficiency is improved.
Detailed Description
The invention provides a method for cleaning an indium phosphide polycrystal material, which comprises the following steps:
sequentially immersing the indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then performing ultrasonic cleaning in water, and finally dehydrating and drying to finish cleaning;
the volume concentration of the bromomethanol is 2-5%, and the cleaning time is 30-60 s; the concentration of the hydrofluoric acid solution is 0.5-2 mol/L, and the cleaning time is 30-60 min; the concentration of the hydrochloric acid solution is 2-4 mol/L, and the cleaning time is 10-30 min.
The method comprises the steps of firstly placing the indium phosphide polycrystal material to be cleaned in a cleaning tank containing a bromomethanol solution, ensuring that the bromomethanol solution can completely submerge the indium phosphide polycrystal material, continuously and gently stirring the solution, and fully contacting the solution with the indium phosphide polycrystal material for soaking and cleaning to corrode the indium phosphide polycrystal material.
In the invention, in the production or processing process of the indium phosphide polycrystal material, some holes, gaps and edge corners are inevitably generated, the indium phosphide polycrystal material cannot be completely polished smooth by using sand paper, impurities and oxide layers in the holes and the gaps cannot be cleaned by using the conventional cleaning process, and the protruding parts such as the corners are easy to damage and scratch a crucible for indium phosphide monocrystal charging, thereby causing serious influence on the next procedure. After the indium phosphide polycrystal material is corroded by adding the bromomethanol solution, the solution can clean and corrode parts, such as edges, scratches, holes, gaps and the like, on the surface of the indium phosphide polycrystal material, which cannot be polished by using abrasive paper or cannot be polished completely, along with the continuous stirring of the solution, so that the indium phosphide polycrystal material is polished smoothly.
In the invention, the bromomethanol solution is prepared from UP grade bromine and methanol, and the volume concentration of the bromomethanol solution is preferably 2-5%, and more preferably 3-4%; such as 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, preferably a range value with any of the above values as upper or lower limits; the cleaning time is preferably 30-60 s, more preferably 40-50 s, such as 30s, 35s, 40s, 45s, 50s, 55s, 60s, and preferably any of the above values is used as an upper limit or a lower limit.
In addition, after the indium phosphide polycrystal material is processed, organic impurities such as grease, wax and the like are attached to the surface of the indium phosphide polycrystal material, the indium phosphide polycrystal material has the function of covering other inorganic impurities, the indium phosphide polycrystal material is easy to carbonize under the high-temperature condition, the generated product is attached to the surface of the polycrystal material and is not easy to remove, and the organic impurities such as grease, wax and the like on the surface of the indium phosphide polycrystal material can be effectively cleaned by using bromomethanol.
Washing the indium phosphide polycrystal material cleaned by using the bromomethanol solution with deionized water for 2-3 times, then placing the indium phosphide polycrystal material into a cleaning tank with an HF solution to ensure that the HF solution can completely submerge the indium phosphide polycrystal material, continuously stirring the HF solution during the washing process, and enabling the HF solution and the SiO on the surface of the crystal bar to be mixed2And reacting to remove Si element.
The InP polycrystal material contacts the quartz piece for a long time in the growth process, and the Si element is generally SiO2The quartz slag is attached to the crystal bar, and quartz slag can easily fall into holes and gaps of the crystal bar during tube cutting and demoulding, so that the crystal bar cannot be cleaned up. The cleaning solution of the existing cleaning process cannot treat the quartz, so that the content of Si element is still high after cleaning is finished, and the quality of the product is influenced.
In the invention, the concentration of the HF solution is preferably 0.5-2 mol/L, more preferably 1-1.5 mol/L, such as 0.5mol/L, 1mol/L, 1.5mol/L, 2mol/L, and preferably a range value with any value as an upper limit or a lower limit; the cleaning time is preferably 30-60 min, and more preferably 40-50 min.
The indium phosphide polycrystal material cleaned by the HF is washed for 2-3 times by using deionized water and then enters an HCl solution, so that the HCl solution is ensured to completely submerge the indium phosphide polycrystal material, the HCl solution is continuously stirred during the process, an oxide layer and metal impurities can be cleaned in a short time, and meanwhile, the HCl solution has a good cleaning effect on S impurity elements.
During the processes of pipe cutting, transportation and processing, the indium phosphide polycrystal material forms a compact oxide layer on the surface, and is difficult to be stained with metal impurities, ammonia water and hydrogen peroxide are added in the existing cleaning process, the reaction time with the metal impurities is long, and the efficiency is low. If HCl is used for cleaning in the second step, not only Si element cannot be cleaned, but also SiO2Other covered impurities cannot be cleaned, so that the cleaning efficiency is influenced, and the second step needs to be cleaned by HF acid.
In the invention, the concentration of the HCl solution is preferably 2-4 mol/L, more preferably 2.5-3.5 mol/L, such as 2mol/L, 2.5mol/L, 3mol/L, 3.5mol/L, 4mol/L, and preferably a range value with any value as an upper limit or a lower limit; the cleaning time is preferably 10-30 min, and more preferably 20-25 min.
The indium phosphide polycrystal material cleaned by HCl is placed in an ultrasonic cleaning tank filled with deionized water for ultrasonic treatment, an ultrasonic cleaning machine converts sound energy of a power ultrasonic frequency source into mechanical vibration through a transducer, ultrasonic waves are radiated to cleaning liquid in the cleaning tank through a cleaning tank wall, and micro bubbles in liquid in the cleaning tank can keep vibrating under the action of the sound waves due to the radiation of the ultrasonic waves. The adsorption of impurities and the surface of the indium phosphide polycrystal material is destroyed, the fatigue destruction of the impurities is caused to be separated, and the vibration of the gas bubbles scrubs the surface of the indium phosphide polycrystal material.
In the invention, the frequency of the ultrasonic wave is preferably 30-50 Hz, more preferably 40Hz, and the time of the ultrasonic wave is preferably 30-60 min, more preferably 40-50 min. The temperature of the ultrasonic wave is preferably 40-70 ℃, and more preferably 50-60 ℃. The ultrasonic operation is preferably carried out for 3-5 times, and after each time, the deionized water is replaced for the next time.
And soaking the ultrasonically treated indium phosphide polycrystal material in UP-grade absolute ethyl alcohol for 2-5 min for dehydration, then blowing the polycrystal material to dry by using high-purity nitrogen, and baking the polycrystal material in a vacuum box for later use.
The invention provides a method for cleaning an indium phosphide polycrystal material, which comprises the following steps: adding indium phosphideThe crystal material is sequentially immersed into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then ultrasonic cleaning is carried out in water, and finally dehydration and drying are carried out to finish cleaning; the volume concentration of the bromomethanol is 2-5%, and the cleaning time is 30-60 s; the concentration of the hydrofluoric acid solution is 0.5-2 mol/L, and the cleaning time is 30-60 min; the concentration of the hydrochloric acid solution is 2-4 mol/L, and the cleaning time is 10-30 min. According to the invention, the bromomethanol is used for corroding and cleaning gaps and holes which cannot be polished by some abrasive paper, so that the subsequent cleaning steps are facilitated; the second step is to clean with HF acid, the InP polycrystal material contacts the quartz piece for a long time in the growth process, and the Si element is generally SiO2The form of the crystal rod is tightly covered on the outer surface of the crystal rod, which influences the cleaning of other impurities, and HF acid is needed to firstly clean SiO on the outer surface of the crystal rod2And (5) cleaning. The third step is to wash with HCl and to form SiO on the surface2After the cleaning, HCl can rapidly react with other impurity elements, so that other impurities can be cleaned in a short time, the cleaning time is greatly shortened compared with 15 hours in the original cleaning process, and the working efficiency is improved.
In order to further illustrate the present invention, the following will describe the cleaning method of the indium phosphide polycrystal material provided by the present invention in detail with reference to the examples, but it should not be construed as limiting the scope of the present invention.
Example 1
Step 1: taking 30kg of indium phosphide polycrystal material, putting the indium phosphide polycrystal material into a cleaning tank 1, preparing a 5 vol% bromomethanol solution by using UP grade bromine and methanol, pouring the solution into the cleaning tank 1, wherein the bromomethanol solution is required to submerge the indium phosphide polycrystal material, continuously stirring the bromomethanol solution to fully contact the solution with the polycrystal material, taking out the indium phosphide polycrystal material after 60 seconds, and washing the indium phosphide polycrystal material for 3 times by using deionized water;
step 2: putting the indium phosphide polycrystal material cleaned in the step (1) into a cleaning tank (2), preparing 2mol/L HF solution by using UP-grade hydrofluoric acid and deionized water, pouring the solution into the cleaning tank (2) to ensure that the HF solution is over the indium phosphide polycrystal material, continuously stirring the HF solution to fully contact the solution with the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and washing for 3 times by using the deionized water;
and step 3: putting the indium phosphide polycrystal material cleaned in the step 2 into a cleaning tank 3, preparing 4mol/L HCl solution by using UP-grade hydrochloric acid and deionized water, pouring the solution into the cleaning tank 3 to ensure that the HCl solution is over the indium phosphide polycrystal material, continuously stirring the HCl solution to fully contact the polycrystal material, soaking and cleaning for 30 minutes, taking out the indium phosphide polycrystal material, and washing for 3 times by using the deionized water;
and 4, step 4: putting the indium phosphide polycrystal material cleaned in the step (3) into an ultrasonic cleaning tank, taking deionized water as a medium, setting the temperature to be 70 ℃, carrying out ultrasonic cleaning for 3 times, wherein each time is 60 minutes, and after each ultrasonic cleaning is finished, replacing the deionized water and carrying out next ultrasonic cleaning operation;
and 5: and after the ultrasonic treatment is finished, taking out the indium phosphide polycrystal material, putting the indium phosphide polycrystal material into a cleaning tank 4, pouring UP-grade absolute ethyl alcohol for soaking for 3min for dehydration, taking out the indium phosphide polycrystal material, drying the indium phosphide polycrystal material by using high-purity nitrogen, and putting the indium phosphide polycrystal material into an oven for drying for later use.
Comparative example 1
The comparative example was carried out by reducing the HCl cleaning process steps in the examples, and the specific operations were as follows:
step 1: taking 30kg of indium phosphide polycrystal material, putting the indium phosphide polycrystal material into a cleaning tank 1, preparing a 5 vol% bromomethanol solution by using UP grade bromine and methanol, pouring the bromomethanol solution into the cleaning tank 1, wherein the bromomethanol solution is required to be higher than the indium phosphide polycrystal material, continuously stirring the bromomethanol solution to fully contact the solution with the polycrystal material, taking out the indium phosphide polycrystal material after 60 seconds, and washing the indium phosphide polycrystal material for 3 times by using deionized water;
step 2: putting the indium phosphide polycrystal material cleaned in the step (1) into a cleaning tank (2), preparing 2mol/L HF solution by using UP-grade hydrofluoric acid and deionized water, pouring the solution into the cleaning tank (2) to ensure that the HF solution is over the indium phosphide polycrystal material, continuously stirring the HF solution to fully contact the solution with the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and washing for 3 times by using the deionized water;
and step 3: putting the indium phosphide polycrystal material cleaned in the step 2 into an ultrasonic cleaning tank, taking deionized water as a medium, setting the temperature to be 70 ℃, carrying out ultrasonic cleaning for 3 times, wherein each time is 60 minutes, and after each ultrasonic cleaning is finished, replacing the deionized water and carrying out the next ultrasonic cleaning operation;
and 4, step 4: and after the ultrasonic treatment is finished, taking out the indium phosphide polycrystal material, putting the indium phosphide polycrystal material into a cleaning tank 4, pouring UP-grade absolute ethyl alcohol for soaking for 3min for dehydration, taking out the indium phosphide polycrystal material, drying the indium phosphide polycrystal material by using high-purity nitrogen, and putting the indium phosphide polycrystal material into an oven for drying for later use.
Comparative example 2
The comparative example is carried out by reducing the steps of the HF cleaning process in the example, and the specific operations are as follows:
step 1: taking 30kg of indium phosphide polycrystal material, putting the indium phosphide polycrystal material into a cleaning tank 1, preparing a 5 vol% bromomethanol solution by using UP grade bromine and methanol, pouring the solution into the cleaning tank 1, wherein the bromomethanol solution is required to submerge the indium phosphide polycrystal material, continuously stirring the bromomethanol solution to fully contact the solution with the polycrystal material, taking out the indium phosphide polycrystal material after 60 seconds, and washing the indium phosphide polycrystal material for 3 times by using deionized water;
step 2: putting the indium phosphide polycrystal material cleaned in the step 1 into a cleaning tank 3, preparing 4mol/L HCl solution by using UP-grade hydrochloric acid and deionized water, pouring the HCl solution into the cleaning tank 3 to ensure that the HCl solution is not covered by the indium phosphide polycrystal material, continuously stirring the HCl solution to fully contact the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and washing for 3 times by using the deionized water;
and 4, step 4: putting the indium phosphide polycrystal material cleaned in the step 2 into an ultrasonic cleaning tank, taking deionized water as a medium, setting the temperature to be 70 ℃, carrying out ultrasonic cleaning for 3 times, wherein each time is 60 minutes, and after each ultrasonic cleaning is finished, replacing the deionized water and carrying out the next ultrasonic cleaning operation;
and 5: and after the ultrasonic treatment is finished, taking out the indium phosphide polycrystal material, putting the indium phosphide polycrystal material into a cleaning tank 4, pouring UP-grade absolute ethyl alcohol for soaking for 3min for dehydration, taking out the indium phosphide polycrystal material, drying the indium phosphide polycrystal material by using high-purity nitrogen, and putting the indium phosphide polycrystal material into an oven for drying for later use.
Comparative example 3
The comparative example is carried out by adopting the cleaning process steps for reducing the bromomethanol in the example, and the specific operation is as follows:
step 1: taking 30kg of indium phosphide polycrystal material, putting the indium phosphide polycrystal material into a cleaning tank 2, preparing 2mol/L HF solution by using UP-grade hydrofluoric acid and deionized water, pouring the HF solution into the cleaning tank 2 to ensure that the HF solution is over the indium phosphide polycrystal material, continuously stirring the HF solution to fully contact the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and washing for 3 times by using deionized water;
step 2: putting the indium phosphide polycrystal material cleaned in the step 1 into a cleaning tank 3, preparing 4mol/L HCl solution by using UP-grade hydrochloric acid and deionized water, pouring the HCl solution into the cleaning tank 3 to ensure that the HCl solution is not covered by the indium phosphide polycrystal material, continuously stirring the HCl solution to fully contact the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and washing for 3 times by using the deionized water;
and step 3: putting the indium phosphide polycrystal material cleaned in the step 2 into an ultrasonic cleaning tank, taking deionized water as a medium, setting the temperature to be 70 ℃, carrying out ultrasonic cleaning for 3 times, wherein each time is 60 minutes, and after each ultrasonic cleaning is finished, replacing the deionized water and carrying out the next ultrasonic cleaning operation;
and 4, step 4: and after the ultrasonic treatment is finished, taking out the indium phosphide polycrystal material, putting the indium phosphide polycrystal material into a cleaning tank 4, pouring UP-grade absolute ethyl alcohol for soaking for 3min for dehydration, taking out the indium phosphide polycrystal material, drying the indium phosphide polycrystal material by using high-purity nitrogen, and putting the indium phosphide polycrystal material into an oven for drying for later use.
Comparative example 4
The comparative example is carried out by adopting the original indium phosphide polycrystal material cleaning process, and the specific operation is as follows:
step 1: taking 30kg of indium phosphide polycrystal material, washing with deionized water or brushing with a small brush to remove black glue on the surface of the indium phosphide polycrystal material, then soaking in acetic acid at 70 ℃ to remove the glue, and then polishing with 100-mesh carborundum paper to remove surface traces to obtain a crude product;
step 2: and (3) soaking the crude product in a mixed solvent consisting of ammonia water, hydrogen peroxide and deionized water for 2 hours, taking out, washing with the deionized water, ultrasonically cleaning for 20 minutes, then putting into an open container containing methanol for cleaning, taking out, airing and evaporating the methanol to obtain the cleaned indium phosphide polycrystal material. In the mixed solvent, the mass fraction of ammonia water is 28-35%, and the mass fraction of hydrogen peroxide is 30-35%.
The washed indium phosphide polycrystal materials of example 1, comparative example 2, comparative example 3 and comparative example 4 were subjected to GDMS analysis, and the analysis results, the appearance comparison and the washing time were as shown in table 1:
TABLE 1 analysis of cleaning results of inventive and comparative examples
As can be seen from the above table:
1. comparative example 1 reduces the cleaning process step of HCl, except for Si element, other impurity elements are generally higher;
2. comparative example 2 reduces the cleaning process steps of HF because SiO2 cannot be effectively removed and has a covering effect on other impurity elements, and therefore other impurity elements cannot be cleaned;
3. comparative example 3 reduces the cleaning process steps of bromomethanol, the hole cracks are not polished smooth, the impurities in the hole cracks cannot be thoroughly cleaned, and the impurity content is higher;
4. the comparative example 4 adopts the original cleaning process, so that the impurity content is high, the cleaning time is long, and the efficiency is low;
5. the embodiment 1 adopts the complete cleaning process, has low impurity content, smooth surface without edges and corners, does not influence the subsequent procedures, and has short cleaning time.
In conclusion, the cleaning process steps in the invention are all indispensable, and compared with the first, second, third and fourth comparative examples, the cleaning process disclosed by the invention has the advantages that the content of impurity elements is greatly reduced, the appearance is polished smoothly, the subsequent charging process is not influenced, the whole cleaning time is greatly shortened, and the working efficiency is improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A method for cleaning an indium phosphide polycrystal material comprises the following steps:
sequentially immersing the indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then performing ultrasonic cleaning in water, and finally dehydrating and drying to finish cleaning;
the volume concentration of the bromomethanol is 2-5%, and the cleaning time is 30-60 s; the concentration of the hydrofluoric acid solution is 0.5-2 mol/L, and the cleaning time is 30-60 min; the concentration of the hydrochloric acid solution is 2-4 mol/L, and the cleaning time is 10-30 min.
2. The cleaning method according to claim 1, wherein the indium phosphide polycrystal material is washed with deionized water 2 to 5 times after being washed with bromomethanol, a hydrofluoric acid solution and a hydrochloric acid solution.
3. The cleaning method according to claim 1, wherein the frequency of the ultrasonic waves is 30 to 50 Hz.
4. The cleaning method according to claim 3, wherein the ultrasonic cleaning is performed 3 to 5 times, and the time of each ultrasonic cleaning is 30 to 60 min.
5. The cleaning method according to claim 4, wherein the temperature of the ultrasonic cleaning is 40 to 70 ℃.
6. The cleaning method according to claim 1, wherein the dehydration is performed by soaking the indium phosphide polycrystal material in absolute ethyl alcohol for 2-5 min.
7. The cleaning method according to claim 1, wherein the cleaning with the bromomethanol, the hydrofluoric acid solution, and the hydrochloric acid solution is performed under stirring.
8. The cleaning method according to claim 1, wherein the drying is performed by blow-drying with high purity nitrogen gas and then drying.
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| JP2000138198A (en) * | 1998-08-28 | 2000-05-16 | Mitsubishi Materials Silicon Corp | Method for cleaning of semiconductor substrate |
| JP2015106647A (en) * | 2013-11-29 | 2015-06-08 | 株式会社Sumco | Method of manufacturing silicon wafer |
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