CN114669546B - Method for cleaning indium phosphide polycrystal material - Google Patents
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- CN114669546B CN114669546B CN202210403210.XA CN202210403210A CN114669546B CN 114669546 B CN114669546 B CN 114669546B CN 202210403210 A CN202210403210 A CN 202210403210A CN 114669546 B CN114669546 B CN 114669546B
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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
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Abstract
The invention provides a method for cleaning indium phosphide polycrystal material, which comprises the following steps: and immersing the indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution in sequence for cleaning, then carrying out 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 the abrasive paper, so that the subsequent cleaning steps are convenient; the second step is to clean the crystal bar with HF acid to obtain SiO on the surface of the crystal bar 2 Cleaning. The third step is to clean with HCl, and SiO is on the surface 2 After cleaning, HCl can react with other impurity elements rapidly, so that other impurities can be cleaned in a short time, and compared with the prior cleaning process, the cleaning time is shortened greatly, and the working efficiency is improved.
Description
Technical Field
The invention belongs to the technical field of semiconductor materials, and particularly relates to a cleaning method of indium phosphide polycrystal material.
Background
Indium phosphide is a group III-V compound semiconductor formed by combining group IIIA indium In and group VA P. Along with the gradual development of application requirements of photoelectrons, microelectronic devices and the like, the excellent performance of the indium phosphide material is also gradually highlighted, and particularly in the field of optical fiber communication, only the indium phosphide semiconductor technology can integrate the functions of a light detector and a laser with other analog and mixed signals on the same substrate, and the indium phosphide semiconductor technology has the advantages of high integration level and low price, so that the optical device realizes great breakthrough; in the wireless field, indium phosphide amplifiers have been greatly improved in many respects, including improved performance and reduced power consumption; in millimeter wave applications where other semiconductor materials such as indium arsenide and silicon are not available, passive imaging and other latest applications can be easily realized through indium phosphide devices.
In the production process of the indium phosphide single crystal, a large amount of indium phosphide polycrystal material is required to be input, the indium phosphide polycrystal material is inevitably bumped in the growth and processing processes, surface pits and cracks are caused, the surface is oxidized or some grease and metal impurities are introduced, the growth of the indium phosphide single crystal is seriously influenced, and the yield is low, so that 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 monocrystal product and reducing the cost.
The existing cleaning process of the indium phosphide polycrystal material generally uses the 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 rods with smooth surfaces can be cleaned, and the crystal rods with holes and cracks can not be treated or cleaned cleanly, and more impurity elements remain in gaps after cleaning, so that the yield of the indium phosphide monocrystal is seriously affected.
Therefore, a new method for cleaning the indium phosphide polycrystal material is needed, the current difficulty is solved, the yield of the indium phosphide monocrystal product is improved, and the cost is reduced.
Disclosure of Invention
The invention aims to provide a method for cleaning indium phosphide polycrystal material, which solves the problems of uncleanness and low cleaning efficiency of the existing process, improves the yield of indium phosphide monocrystal, reduces the production cost and improves the market competitiveness.
The invention provides a method for cleaning indium phosphide polycrystal material, which comprises the following steps:
sequentially immersing indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then carrying out 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 rinsed with deionized water 2 to 5 times after washing with bromomethanol, after washing with a hydrofluoric acid solution and after washing with a hydrochloric acid solution, respectively.
Preferably, the frequency of the ultrasonic wave is 30-50 Hz.
Preferably, ultrasonic cleaning is carried out for 3 to 5 times, and the time of each ultrasonic treatment is 30 to 60 minutes.
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 washing is performed with bromomethanol, hydrofluoric acid solution and hydrochloric acid solution under stirring.
Preferably, the drying is to dry with high-purity nitrogen gas and then dry.
The invention provides a method for cleaning indium phosphide polycrystal material, which comprises the following steps: sequentially immersing indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then carrying out 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 the abrasive paper, so that the subsequent cleaning steps are convenient; the second step is to wash with HF acid, the indium phosphide polycrystal material contacts the quartz piece for a long time in the growth process, and the Si element is generally SiO 2 The form of the alloy is tightly covered on the outer surface of the crystal bar, other impurities are influenced to be cleaned, and the SiO on the outer surface of the crystal bar needs to be firstly cleaned by HF acid 2 Cleaning. The third step is to clean with HCl, and SiO is on the surface 2 After cleaning, HCl can react with other impurity elements rapidly, so that other impurities can be cleaned in a short time, and compared with the prior cleaning process, the cleaning time is shortened greatly, and the working efficiency is improved.
Detailed Description
The invention provides a method for cleaning indium phosphide polycrystal material, which comprises the following steps:
sequentially immersing indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then carrying out 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 with a bromomethanol solution, ensuring that the bromomethanol solution can completely permeate the indium phosphide polycrystal material, continuously lightly stirring the solution, fully contacting the solution with the indium phosphide polycrystal material, and soaking and washing for corrosion.
In the invention, in the production or processing process of the indium phosphide polycrystal material, holes, gaps and edges and corners of the material are inevitably produced, the material cannot be completely polished and smooth by sand paper, impurities and oxide layers in the holes and the gaps cannot be cleaned by the existing cleaning process, protruding parts such as the edges and corners are easy to damage and scratch the crucible for loading the indium phosphide monocrystal, and the crucible has serious influence on the next process. After the solution of bromomethanol is added for corrosion, the solution can clean and corrode places such as corners, scratches, holes and gaps on the surface of the indium phosphide polycrystal material which cannot be polished or cannot be polished thoroughly by sand paper along with continuous stirring of the solution, and the polishing is smooth.
In the invention, the bromomethanol solution is prepared by preparing UP-level bromine and methanol, and the volume concentration of the bromomethanol solution is preferably 2-5%, more preferably 3-4%; such as 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, preferably a range value having any of the above values as an upper limit or a lower limit; the washing time is preferably 30 to 60 seconds, more preferably 40 to 50 seconds, such as 30 seconds, 35 seconds, 40 seconds, 45 seconds, 50 seconds, 55 seconds, 60 seconds, and preferably a range value having any of the above values as an upper limit or a lower limit.
In addition, after the indium phosphide polycrystal material is processed, the surface is attached with organic impurities such as grease and wax, the surface has a covering effect on other inorganic impurities, and the product generated by the method is easy to carbonize under the high-temperature condition, and is not easy to remove when attached to the surface of the polycrystal material.
Flushing the indium phosphide polycrystal material which is cleaned by using the bromomethanol solution with deionized waterAfter 2-3 times of washing, the solution is put into a washing tank with HF solution to ensure that the HF solution can completely permeate the indium phosphide polycrystal material, and the HF solution and SiO on the surface of the crystal bar are continuously stirred during the period 2 And (3) reacting to remove Si element.
The indium phosphide polycrystal material is contacted with a quartz piece for a long time in the growth process, and Si element is generally SiO 2 In the form of being attached to the crystal bar, quartz scraps can easily fall into holes and gaps of the crystal bar in the process of cutting and demolding, and cannot be cleaned. The cleaning liquid of the existing cleaning process cannot treat the quartz, so that the content of Si element is still high after the cleaning is finished, and the quality of a product is affected.
In the present invention, the concentration of the HF solution is preferably 0.5 to 2mol/L, more preferably 1 to 1.5mol/L, such as 0.5mol/L,1mol/L,1.5mol/L,2mol/L, preferably a range value having any of the above values as an upper limit or a lower limit; the washing time is preferably 30 to 60 minutes, more preferably 40 to 50 minutes.
After the HF-cleaned indium phosphide polycrystal material is washed for 2-3 times by deionized water, the HF-cleaned indium phosphide polycrystal material enters an HCl solution, so that the HCl solution can completely permeate 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.
In the process of cutting, transporting and processing the indium phosphide polycrystal material, a compact oxide layer is formed on the surface, and the indium phosphide polycrystal material is inevitably 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 the second step is performed by HCl, the Si element cannot be cleaned, and the SiO is 2 Other impurities covered cannot be cleaned, so that the cleaning efficiency is affected, and therefore, the second step needs to be cleaned by HF acid.
In the present invention, the concentration of the HCl solution is preferably 2 to 4mol/L, more preferably 2.5 to 3.5mol/L, such as 2mol/L,2.5mol/L,3mol/L,3.5mol/L,4mol/L, preferably a range value having any of the above values as an upper limit or a lower limit; the washing time is preferably 10 to 30 minutes, more preferably 20 to 25 minutes.
The method comprises the steps of placing indium phosphide polycrystal material cleaned by HCl into an ultrasonic cleaning tank filled with deionized water for ultrasonic treatment, converting the acoustic energy of a power ultrasonic frequency source into mechanical vibration by an ultrasonic cleaning machine through a transducer, radiating ultrasonic waves to cleaning liquid in the cleaning tank through a cleaning tank wall, and enabling microbubbles in the liquid in the cleaning tank to keep vibrating under the action of the acoustic wave due to the radiation of the ultrasonic waves. Destroying the adsorption of impurities and the surface of the indium phosphide polycrystal material, causing the fatigue fracture of the impurities to be separated, and scrubbing the surface of the indium phosphide polycrystal material by the vibration of gas bubbles.
In the present invention, the frequency of the ultrasonic wave is preferably 30 to 50Hz, more preferably 40Hz, and the time of the ultrasonic wave is preferably 30 to 60min, more preferably 40 to 50min. The temperature of the ultrasound is preferably 40 to 70 ℃, more preferably 50 to 60 ℃. The ultrasonic operation is preferably carried out for 3 to 5 times, and deionized water is replaced after each ultrasonic operation is finished and then the ultrasonic operation is carried out for the next time.
The indium phosphide polycrystal material after ultrasonic treatment is soaked in UP level absolute ethyl alcohol for 2-5 min for dewatering operation, and then is dried by high-purity nitrogen gas, and is put into a vacuum box for baking for standby.
The invention provides a method for cleaning indium phosphide polycrystal material, which comprises the following steps: sequentially immersing indium phosphide polycrystal material into bromomethanol, hydrofluoric acid solution and hydrochloric acid solution for cleaning, then carrying out 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 the abrasive paper, so that the subsequent cleaning steps are convenient; the second step is to wash with HF acid, the indium phosphide polycrystal material contacts the quartz piece for a long time in the growth process, and the Si element is generally SiO 2 The form of the alloy is tightly covered on the outer surface of the crystal bar, other impurities are influenced to be cleaned, and the SiO on the outer surface of the crystal bar needs to be firstly cleaned by HF acid 2 Cleaning. The third step is to clean with HCl, and SiO is on the surface 2 After cleaning, HCl can react with other impurity elements rapidly to make otherThe impurities are cleaned in a short time, compared with the prior cleaning process, the cleaning time is shortened greatly by 15 hours, and the working efficiency is improved.
In order to further illustrate the present invention, the following examples are provided to illustrate a method for cleaning an indium phosphide polycrystal material according to the present invention, but the present invention is not limited thereto.
Example 1
Step 1: taking 30kg of indium phosphide polycrystal material, placing the indium phosphide polycrystal material into a cleaning tank 1, preparing 5vol% of bromomethanol solution by using UP-level bromine and methanol, pouring the bromomethanol solution into the cleaning tank 1, continuously stirring the bromomethanol solution to ensure that the solution is fully contacted with the polycrystal material, taking out the indium phosphide polycrystal material after 60 seconds, and flushing the indium phosphide polycrystal material with deionized water for 3 times;
step 2: placing the indium phosphide polycrystal material cleaned in the step 1 into a cleaning tank 2, preparing 2mol/L HF solution by using UP-level hydrofluoric acid and deionized water, pouring the solution into the cleaning tank 2, ensuring that the HF solution is not over the indium phosphide polycrystal material, continuously stirring the HF solution to ensure that the solution is fully contacted with the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and flushing the indium phosphide polycrystal material with deionized water for 3 times;
step 3: placing the indium phosphide polycrystal material cleaned in the step 2 into a cleaning tank 3, preparing 4mol/L HCl solution by using UP-level hydrochloric acid and deionized water, pouring the solution into the cleaning tank 3, ensuring that the HCl solution is over the indium phosphide polycrystal material, continuously stirring the HCl solution to ensure that the solution is fully contacted with the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and flushing the indium phosphide polycrystal material with deionized water for 3 times;
step 4: placing the indium phosphide polycrystal material cleaned in the step 3 into an ultrasonic cleaning tank, using deionized water as a medium, setting the temperature to 70 ℃, performing ultrasonic cleaning for 3 times, each time for 60 minutes, and replacing the deionized water after each ultrasonic cleaning is completed, and performing the next ultrasonic cleaning operation;
step 5: after the ultrasonic treatment is completed, taking out the indium phosphide polycrystal material, putting the material into a cleaning tank 4, pouring UP level absolute ethyl alcohol into the tank to soak for 3min for dehydration operation, taking out the material, drying the material by high-purity nitrogen, and putting the material into an oven for drying for standby.
Comparative example 1
The comparative example was performed using the reduced HCl rinse process step of the example, and the specific procedure was as follows:
step 1: taking 30kg of indium phosphide polycrystal material, placing the indium phosphide polycrystal material into a cleaning tank 1, preparing 5vol% of bromomethanol solution by using UP-level bromine and methanol, pouring the bromomethanol solution into the cleaning tank 1, continuously stirring the bromomethanol solution to ensure that the solution is fully contacted with the polycrystal material, taking out the indium phosphide polycrystal material after 60 seconds, and flushing the indium phosphide polycrystal material with deionized water for 3 times;
step 2: placing the indium phosphide polycrystal material cleaned in the step 1 into a cleaning tank 2, preparing 2mol/L HF solution by using UP-level hydrofluoric acid and deionized water, pouring the solution into the cleaning tank 2, ensuring that the HF solution is not over the indium phosphide polycrystal material, continuously stirring the HF solution to ensure that the solution is fully contacted with the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and flushing the indium phosphide polycrystal material with deionized water for 3 times;
step 3: placing the indium phosphide polycrystal material cleaned in the step 2 into an ultrasonic cleaning tank, using deionized water as a medium, setting the temperature to 70 ℃, performing ultrasonic cleaning for 3 times, each time for 60 minutes, and replacing the deionized water after each ultrasonic cleaning is completed, and performing the next ultrasonic cleaning operation;
step 4: after the ultrasonic treatment is completed, taking out the indium phosphide polycrystal material, putting the material into a cleaning tank 4, pouring UP level absolute ethyl alcohol into the tank to soak for 3min for dehydration operation, taking out the material, drying the material by high-purity nitrogen, and putting the material into an oven for drying for standby.
Comparative example 2
The comparative example was performed using the reduced HF cleaning process steps of the examples, and the specific operations are as follows:
step 1: taking 30kg of indium phosphide polycrystal material, placing the indium phosphide polycrystal material into a cleaning tank 1, preparing 5vol% of bromomethanol solution by using UP-level bromine and methanol, pouring the bromomethanol solution into the cleaning tank 1, continuously stirring the bromomethanol solution to ensure that the solution is fully contacted with the polycrystal material, taking out the indium phosphide polycrystal material after 60 seconds, and flushing the indium phosphide polycrystal material with deionized water for 3 times;
step 2: placing the indium phosphide polycrystal material cleaned in the step 1 into a cleaning tank 3, preparing 4mol/L HCl solution by using UP-level hydrochloric acid and deionized water, pouring the solution into the cleaning tank 3, ensuring that the HCl solution is over the indium phosphide polycrystal material, continuously stirring the HCl solution to ensure that the solution is fully contacted with the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and flushing the indium phosphide polycrystal material with deionized water for 3 times;
step 4: placing the indium phosphide polycrystal material cleaned in the step 2 into an ultrasonic cleaning tank, using deionized water as a medium, setting the temperature to 70 ℃, performing ultrasonic cleaning for 3 times, each time for 60 minutes, and replacing the deionized water after each ultrasonic cleaning is completed, and performing the next ultrasonic cleaning operation;
step 5: after the ultrasonic treatment is completed, taking out the indium phosphide polycrystal material, putting the material into a cleaning tank 4, pouring UP level absolute ethyl alcohol into the tank to soak for 3min for dehydration operation, taking out the material, drying the material by high-purity nitrogen, and putting the material into an oven for drying for standby.
Comparative example 3
The comparative example was carried out using the reduced bromomethanol cleaning procedure of the examples, and the specific procedure is as follows:
step 1: taking 30kg of indium phosphide polycrystal material, placing the indium phosphide polycrystal material into a cleaning tank 2, preparing 2mol/L HF solution by using UP-level hydrofluoric acid and deionized water, pouring the solution into the cleaning tank 2, ensuring that the HF solution is not over the indium phosphide polycrystal material, continuously stirring the HF solution to ensure that the solution is fully contacted with the polycrystal material, taking out the indium phosphide polycrystal material after soaking and washing for 30 minutes, and flushing the indium phosphide polycrystal material with deionized water for 3 times;
step 2: placing the indium phosphide polycrystal material cleaned in the step 1 into a cleaning tank 3, preparing 4mol/L HCl solution by using UP-level hydrochloric acid and deionized water, pouring the solution into the cleaning tank 3, ensuring that the HCl solution is over the indium phosphide polycrystal material, continuously stirring the HCl solution to ensure that the solution is fully contacted with the polycrystal material, taking out the indium phosphide polycrystal material after soaking and cleaning for 30 minutes, and flushing the indium phosphide polycrystal material with deionized water for 3 times;
step 3: placing the indium phosphide polycrystal material cleaned in the step 2 into an ultrasonic cleaning tank, using deionized water as a medium, setting the temperature to 70 ℃, performing ultrasonic cleaning for 3 times, each time for 60 minutes, and replacing the deionized water after each ultrasonic cleaning is completed, and performing the next ultrasonic cleaning operation;
step 4: after the ultrasonic treatment is completed, taking out the indium phosphide polycrystal material, putting the material into a cleaning tank 4, pouring UP level absolute ethyl alcohol into the tank to soak for 3min for dehydration operation, taking out the material, drying the material by high-purity nitrogen, and putting the material into an oven for drying for standby.
Comparative example 4
The comparative example is carried out by adopting an original indium phosphide polycrystal material cleaning process, and the specific operation is as follows:
step 1: taking 30kg of indium phosphide polycrystal material, flushing 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 diamond sand paper to remove surface marks 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, flushing with deionized water, ultrasonically cleaning for 20 minutes, then placing the crude product in an open container for 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 indium phosphide polycrystal materials washed in example 1, comparative example 2, comparative example 3 and comparative example 4 were sampled respectively for GDMS analysis, and the analysis results, appearance comparison and washing time are shown in Table 1:
TABLE 1 analysis of cleaning results for inventive and comparative examples
As can be seen from the table above:
1. comparative example 1 reduced HCl rinse process step, other impurity elements besides Si element are generally higher;
2. comparative example 2 reduces the HF cleaning process step because SiO2 cannot be removed effectively, 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 smoothly, impurities in the holes cannot be thoroughly cleaned, and the impurity content is higher;
4. the comparative example 4 adopts the original cleaning process, has high impurity content, long cleaning time and low efficiency;
5. the embodiment 1 adopts the complete cleaning process of the invention, has low impurity content, smooth surface and no edges and corners, does not influence the subsequent process and has short cleaning time.
In summary, the cleaning process steps in the invention are not indispensable, compared with the first, second, third and fourth comparative examples, the impurity element content is greatly reduced, the appearance is polished smooth, the subsequent charging process is not influenced, the whole cleaning time is also greatly shortened, and the working efficiency is improved.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (5)
1. The method for cleaning the 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 carrying out ultrasonic cleaning for 3-5 times in water, wherein the time of each ultrasonic treatment is 30-60 min, and finally dehydrating and drying to finish cleaning;
the volume concentration of 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 ultrasonic frequency is 30-50 Hz, and the ultrasonic cleaning temperature is 40-70 ℃.
2. The cleaning method according to claim 1, wherein the indium phosphide polycrystal material is rinsed with deionized water 2 to 5 times after the cleaning with bromomethanol, after the cleaning with a hydrofluoric acid solution and after the cleaning with a hydrochloric acid solution, respectively.
3. The method according to claim 1, wherein the dehydration is performed by immersing the indium phosphide polycrystal material in absolute ethanol for 2 to 5 minutes.
4. The method according to claim 1, wherein the washing is performed with bromomethanol, hydrofluoric acid solution and hydrochloric acid solution under stirring.
5. The method according to claim 1, wherein the drying is performed by drying with high-purity nitrogen gas and then drying.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110834228A (en) * | 2019-11-28 | 2020-02-25 | 湖南大合新材料有限公司 | Cleaning process of quartz tube for growing tellurium-zinc-cadmium |
| CN112382555A (en) * | 2020-11-12 | 2021-02-19 | 广东先导先进材料股份有限公司 | Method for cleaning indium phosphide substrate |
| CN113000476A (en) * | 2021-01-26 | 2021-06-22 | 威科赛乐微电子股份有限公司 | Gallium arsenide material cleaning process |
| CN113793801A (en) * | 2021-09-07 | 2021-12-14 | 广东先导微电子科技有限公司 | Method for cleaning indium phosphide substrate wafer |
| CN114220732A (en) * | 2022-02-23 | 2022-03-22 | 北京通美晶体技术股份有限公司 | Ultra-clean cleaning method and application of indium phosphide wafer |
-
2022
- 2022-04-18 CN CN202210403210.XA patent/CN114669546B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110834228A (en) * | 2019-11-28 | 2020-02-25 | 湖南大合新材料有限公司 | Cleaning process of quartz tube for growing tellurium-zinc-cadmium |
| CN112382555A (en) * | 2020-11-12 | 2021-02-19 | 广东先导先进材料股份有限公司 | Method for cleaning indium phosphide substrate |
| CN113000476A (en) * | 2021-01-26 | 2021-06-22 | 威科赛乐微电子股份有限公司 | Gallium arsenide material cleaning process |
| CN113793801A (en) * | 2021-09-07 | 2021-12-14 | 广东先导微电子科技有限公司 | Method for cleaning indium phosphide substrate wafer |
| CN114220732A (en) * | 2022-02-23 | 2022-03-22 | 北京通美晶体技术股份有限公司 | Ultra-clean cleaning method and application of indium phosphide wafer |
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