CN113555274B - Chip cleaning method - Google Patents
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- CN113555274B CN113555274B CN202110827556.8A CN202110827556A CN113555274B CN 113555274 B CN113555274 B CN 113555274B CN 202110827556 A CN202110827556 A CN 202110827556A CN 113555274 B CN113555274 B CN 113555274B
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Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02082—Cleaning product to be cleaned
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
-
- 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
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Cleaning By Liquid Or Steam (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
The invention provides a chip cleaning method, which comprises the following steps: after the chip is subjected to the first baking treatment, cleaning the chip by adopting the first mixed liquid, the second mixed liquid and the two fluids in sequence, and drying the cleaned chip and then carrying out the second baking treatment; the first mixed liquid comprises cold degreasing agent and water, the second mixed liquid comprises cold degreasing agent and water, and the volume concentration of the cold degreasing agent in the second mixed liquid is lower than that of the cold degreasing agent in the first mixed liquid. The chip cleaning method provided by the invention has good cleaning effect, and particularly the core particles after cleaning are not easy to drop and lose, and the surface of the chip has no residual liquid.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a chip cleaning method.
Background
The light emitting diode (Light Emitting Diode, abbreviated as LED) is a semiconductor electronic device for converting electric energy into light energy, the LED chip is a core component for emitting light of the LED, the latter half of the manufacture of the LED chip includes steps of grinding and thinning, scribing, splitting, film pouring, film spreading, spot measurement, sorting and the like, the LED chip is developed towards the direction of refinement and differentiation at the present stage, and how to improve the performance index of the LED chip is always a continuously pursued goal of those skilled in the art.
The LED chip is extremely easy to pollute in the latter half of the manufacture of the LED chip, and main pollutants are derived from the following aspects: firstly, in the process of dicing and wafer breaking, finely-divided particle pollutants appear due to substrate breakage of chips; secondly, organic pollutants are generated due to falling of a blue film on a blue film chip in the film pouring and film expanding processes; thirdly, in the spot measurement process, the probe used for spot measurement oxidizes and falls off to generate metal particle pollutants; fourth, in the separation process, particle pollutants and organic pollutants brought by a suction nozzle used for separation; fifthly, in the storage and transfer processes of the chip, the chip adsorbs suspended particulate pollutants and greasy dirt pollutants in the environment. Therefore, the pollution caused by the pollutants in the preparation process of the LED chip can be greatly influenced, if the pollutants are not treated in time, the reliability and the durability of the LED chip can be greatly influenced, such as the phenomena of electric leakage failure, low light extraction rate and the like of the chip, particularly, if the negative electrode (N) and the positive electrode (P) of the chip are polluted or remained by organic matters, the problems of poor bonding wires and the like can be caused in the subsequent LED chip packaging, so that the chip manufacturing factory can be greatly hidden in quality and economic loss.
Up to now, the industry has gradually realized the harm that the chip pollutes, but along with the size of the LED chip is getting smaller and smaller, the chip is fixed on the carrier (e.g. blue film, UV film) after sorting for the cleaning difficulty of chip increases, and traditional manual chip cleaning method, through two fluids or high-pressure pump cleaning machine to wash the chip, often wash incompletely, causes the core particle loss that drops. In order to improve the chip cleaning efficiency, the prior art gradually develops an automatic chip cleaning device, for example, patent document CN109962028A discloses a full-automatic chip cleaning device and a cleaning process, and the automatic chip cleaning device improves the chip cleaning efficiency, but often causes a large amount of core particles to drop and lose in the chip cleaning process, in addition, the liquid medicine is often not treated cleanly in the chip cleaning process, and the residual liquid medicine brings secondary pollution to the chip, so that the chip cleaning effect is poor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a chip cleaning method, which at least solves the problems of easy drop loss of core particles after cleaning, secondary pollution of chips caused by residual liquid medicine and the like in the prior art.
The invention provides a chip cleaning method, which comprises the following steps: after the chip is subjected to the first baking treatment, cleaning the chip by adopting the first mixed liquid, the second mixed liquid and the two fluids in sequence, and drying the cleaned chip and then carrying out the second baking treatment; the first mixed liquid comprises cold degreasing agent and water, the second mixed liquid comprises cold degreasing agent and water, and the volume concentration of the cold degreasing agent in the second mixed liquid is lower than that of the cold degreasing agent in the first mixed liquid.
According to an embodiment of the present invention, the conditions of the first baking process are: the baking temperature is 25-65 ℃, and the baking time is 300-1800 seconds; and/or, the conditions of the second baking treatment are: the baking temperature is 25-65 ℃, and the baking time is 200-1800 seconds.
According to an embodiment of the invention, the cold degreasing agent comprises at least one of LF-106 cold degreasing agent and HWJ-109 cold degreasing agent.
According to one embodiment of the invention, the volume ratio of the cold degreasing agent to the water in the first mixed solution is 1:1-1:15; and/or the volume ratio of the cold degreasing agent to the water in the second mixed liquid is 1:5-1:25.
According to an embodiment of the present invention, further comprising: after the first mixed solution is adopted for cleaning, two fluids are adopted for cleaning, and then the second mixed solution is adopted for cleaning.
According to one embodiment of the present invention, the cleaning process using the first mixed solution includes: after the chip is soaked in the first mixed solution for 5-80 seconds, brushing the chip; and/or the process of adopting the second mixed solution to carry out the cleaning treatment comprises the following steps: and (3) soaking the chip in the second mixed solution for 5-80 seconds, and then brushing the chip.
According to one embodiment of the invention, a chip automatic cleaning machine is adopted for brushing treatment, the chip automatic cleaning machine comprises a cleaning table and a brush for brushing treatment, the chip is placed on the cleaning table and is brushed by the brush in the brushing treatment process, the rotating speed of the cleaning table is 0-500RPM, and the brushing treatment time is 1-80 seconds.
According to an embodiment of the invention, the two fluids comprise a gas and a liquid; and/or the time for the cleaning treatment with the two fluids is 1-600 seconds.
According to one embodiment of the invention, the chip automatic cleaning machine is used for cleaning, the chip automatic cleaning machine comprises a cleaning table and a first nozzle, the chip is arranged on the cleaning table, the nozzle is used for spraying two fluids on the cleaning table, the rotating speed of the cleaning table is 10-1500RPM in the process of cleaning by adopting the two fluids, the two fluids comprise gas and liquid, the pressure of the liquid is 0.1-0.8MPa, and the flow rate of the liquid is 0.1-0.8L/min.
According to one embodiment of the invention, compressed gas is used for drying, the pressure of the compressed gas is 0.08-0.9MPa, the drying time is 1-600 seconds, and the rotation speed of the chip is controlled to be 100-2500RPM.
The implementation of the invention has at least the following beneficial effects:
according to the chip cleaning method provided by the invention, the adhesion strength of the chip and the carrier can be enhanced through the first baking treatment, the falling of core particles in the subsequent cleaning process can be prevented, the integrity and the quality of the chip can be ensured, the chip is cleaned by adopting the high-proportion cleaning liquid after the first baking treatment, the pollutants on the surface of the chip can be removed to the greatest extent, the cold degreasing agent and the like residues are remained on the surface of the chip after the cleaning treatment of the chip by adopting the high-proportion cleaning agent, the chip is cleaned by adopting the low-proportion cleaning agent, the residues such as the cold degreasing agent on the surface of the chip can be dissolved, the chip is cleaned by adopting the second fluid, and the water vapor of the chip is further removed and the adhesion strength of the chip and the carrier is enhanced after the drying of the cleaned chip. The chip cleaning method can effectively remove pollutants on the surface of the chip, and the cleaned chip surface has no residual cleaning liquid, so that secondary pollution is avoided, the cleaning effect is good, and the method has the advantages of simplicity and convenience in operation and the like, and is particularly suitable for batch cleaning of LED chips.
Drawings
FIG. 1 is a flow chart of a method for cleaning a chip according to an embodiment of the invention;
FIG. 2 is a view showing the whole appearance of the chip after cleaning in embodiment 1 of the present invention;
FIG. 3 is an elemental analysis (EDS) diagram of a cleaned chip according to example 2 of the present invention;
FIG. 4 is an overall external view of the chip after cleaning in comparative example 1 of the present invention;
FIG. 5 is an elemental analysis (EDS) chart of the surface of the chip after cleaning in comparative example 2 of the present invention.
Detailed Description
The present invention will be described in further detail below for the purpose of better understanding of the aspects of the present invention by those skilled in the art.
The chip cleaning method provided by the invention comprises the following steps: after the chip is subjected to the first baking treatment, cleaning the chip by adopting the first mixed liquid, the second mixed liquid and the two fluids in sequence, and drying the cleaned chip and then carrying out the second baking treatment; the first mixed liquid comprises cold degreasing agent and water, the second mixed liquid comprises cold degreasing agent and water, and the volume concentration of the cold degreasing agent in the second mixed liquid is lower than that of the cold degreasing agent in the first mixed liquid.
Specifically, the purpose of the first baking treatment is to enhance the adhesion strength of the chip and the carrier, prevent the loosening and falling of the core particles in the cleaning process, firstly, the mixed reagent of the high-proportion cold degreasing agent and water is used for cleaning the chip, so as to remove pollutants on the surface of the chip, such as metal, dust and other particle pollutants, grease pollutants and the like on the surface of the chip to the greatest extent, but the surface of the chip cleaned by the mixed reagent with the high proportion has residues of cleaning liquid such as the cold degreasing agent, so that the mixed reagent of the low-proportion cold degreasing agent and water is used for dissolving the residues such as the cold degreasing agent on the surface of the chip, and then the two-fluid is used for cleaning the chip, so that the pollutants on the surface of the chip can be effectively removed, and the cleaned surface of the chip does not remain the first mixed liquid, the second mixed liquid and other cleaning liquid, so that secondary pollution cannot occur; and drying the cleaned chip, and then carrying out a second baking treatment on the chip, wherein the purpose of the second baking treatment is to dry a small amount of water (vapor) remained on the chip and further enhance the adhesion strength of the chip and the carrier.
The chip cleaning method is suitable for cleaning the surfaces of chips, particularly cleaning the sorted light-emitting diode chips (LED chips), sorting is generally carried out by distinguishing and sorting the LED chips after spot measurement according to parameter standards such as wavelength, luminous intensity, reverse leakage yield, working voltage and the like, the LED chips are classified into a plurality of grades (Bin) and categories as a result, and then the LED chips are packaged in different bins according to set testing standards through a sorting machine.
The chip has a core particle and a film for fixing or carrying the core particle, such as a blue film, a UV film, etc., and the chip of the present invention may be a chip conventional in the art, such as a chip in which the carrier is a blue film or a UV film.
In the invention, chips can be cleaned in batches, in a specific implementation process, the separated chips can be arranged in different material boxes, wherein each material box can be loaded with 1-50 chips, the material boxes are placed in a baking device (such as an oven or the like) for baking so as to realize the first baking treatment of the chips, then the chips after the baking treatment are cleaned, the cleaned chips are dried, the dried chips can be arranged in different material boxes, and the material boxes are placed in the baking device (such as the oven or the like) for baking so as to realize the second baking treatment of the chips.
Through the first baking treatment, the strength of the chip can be enhanced, for example, the adhesion between the core particles and the film for fixing or bearing the core particles is enhanced, so that the subsequent cleaning treatment is facilitated, the loosening and falling of the core particles in the cleaning process are prevented, and the quality of the cleaned chip is ensured. Specifically, in some preferred embodiments, the temperature of the first bake treatment may be in the range of 25-65 ℃, such as 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃ or any two thereof, and the time of the first bake treatment is in the range of 300-1800 seconds, such as 300 seconds, 400 seconds, 800 seconds, 1000 seconds, 1500 seconds, 1800 seconds or any two thereof.
After drying, a small amount of water vapor generally remains on the chip, and the water vapor remaining on the surface of the chip can be removed through the second baking treatment, so that the strength of the chip is further ensured, the loosening and falling of core particles are avoided, and the quality of the chip after cleaning is ensured. Further, the temperature of the second baking treatment may be 25 to 65 ℃, such as 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃ or any two of them, and the time of the second baking treatment may be 200 to 1800 seconds, such as 200 seconds, 400 seconds, 800 seconds, 1000 seconds, 1500 seconds, 1800 seconds or any two of them.
Typically, the cold degreasing agent is in a liquid state and includes at least one of an alkaline degreasing agent, an emulsion degreasing agent, and a solvent degreasing agent. In some embodiments, the cold degreasing agent comprises at least one of LF-106 cold degreasing agent and HWJ-109 cold degreasing agent, and specifically may be selected from LF-106 cold degreasing agent of Lorentia environmental protection technology Co., ltd, or HWJ-109 cold degreasing agent of Liujia metal technology Co., ltd.
In some embodiments, the volume ratio of cold degreasing agent to water in the first mixed liquor is in the range of 1:1-1:15, e.g., 1:1, 1:3, 1:5, 1:7, 1:8, 1:11, 1:13, 1:15, or any two thereof, and in particular embodiments, the first mixed liquor may be composed of cold degreasing agent and water.
In some embodiments, the volume ratio of cold degreasing agent to water in the second mixed liquor is in the range of 1:5-1:25, e.g., 1:5, 1:7, 1:10, 1:12, 1:15, 1:18, 1:20, 1:25, or any two thereof, and in particular embodiments, the second mixed liquor may be comprised of cold degreasing agent and water.
In some embodiments, further comprising: after the first mixed solution is adopted for cleaning, two fluids are adopted for cleaning, and then the second mixed solution is adopted for cleaning. Specifically, as shown in fig. 1, after the chip is subjected to the first baking treatment, the first mixed solution, the second mixed solution (denoted as first two-fluid), the second mixed solution and the second fluid (denoted as second two-fluid) are sequentially used for cleaning, so that cleaning solution residues such as the first mixed solution, the second mixed solution and the like on the surface of the chip are further removed.
In some embodiments, the two fluids include a gas and a liquid, i.e., the first two fluids may include a gas and a liquid, and the second fluid may include a gas and a liquid, which may be the same or different. Alternatively, the liquid in the two fluids may comprise water, such as deionized water, and the gas may comprise high purity nitrogen.
In some embodiments, the process of performing the cleaning process with the first mixed liquor includes: and (3) after the chip is soaked in the first mixed solution for 5-80 seconds, brushing the chip.
In the specific implementation of the invention, the chip is cleaned by adopting the chip automatic cleaning machine, wherein the chip automatic cleaning machine comprises a cleaning chamber, a cleaning table and at least one spray head, the cleaning table is arranged in the cleaning chamber, and the first spray head is used for spraying first mixed liquid into the cleaning chamber of the cleaning machine and is provided with a pipeline connected with the first mixed liquid. When the chip automatic cleaning machine is used for cleaning, the chip is placed on a cleaning table, the first spray head faces the chip, the first mixed liquid is sprayed on the chip through the first spray head, so that the first mixed liquid submerges the chip, the chip is brushed after being soaked, wherein the spraying time is 3-50 seconds, such as 3 seconds, 8 seconds, 12 seconds, 24 seconds, 48 seconds, 50 seconds or a range formed by any two of the three, and the soaking time is 5-80 seconds, such as 5 seconds, 10 seconds, 20 seconds, 30 seconds, 40 seconds, 50 seconds, 60 seconds, 70 seconds, 80 seconds or a range formed by any two of the three.
In some embodiments, the process of performing the cleaning process with the second mixed liquor includes: and (3) soaking the chip in the second mixed solution for 5-80 seconds, and then brushing the chip.
In the specific implementation of the invention, the chip is cleaned by adopting the chip automatic cleaning machine, wherein the chip automatic cleaning machine comprises a cleaning chamber, a cleaning table and at least one spray head, the cleaning table is arranged in the cleaning chamber, and the second spray head is used for spraying second mixed liquid into the cleaning chamber of the cleaning machine and is provided with a pipeline connected with the second mixed liquid. When the chip automatic cleaning machine is used for cleaning, the chip to be cleaned is placed on the cleaning table, the second spray head faces the chip to be cleaned, the second mixed liquid is sprayed on the chip to be cleaned through the second spray head, so that the second mixed liquid submerges the chip, the chip is scrubbed after being soaked, wherein the spraying time is 3-50 seconds, such as 3 seconds, 8 seconds, 12 seconds, 24 seconds, 48 seconds, 50 seconds or any two of the spraying time, and the soaking time is 5-80 seconds, such as 5 seconds, 10 seconds, 20 seconds, 30 seconds, 40 seconds, 50 seconds, 60 seconds, 70 seconds, 80 seconds or any two of the soaking time.
In some embodiments, a chip automatic cleaner is used for the brushing treatment, the chip automatic cleaner comprises a cleaning table and a brush for the brushing treatment, during the brushing treatment, the chip is placed on the cleaning table and brushed by the brush, the rotation speed of the cleaning table is 0-500RPM, and the brushing treatment time is 1-80 seconds.
Specifically, the automatic chip cleaning machine comprises a cleaning chamber, a cleaning table (or a carrying table) and a brush, wherein the cleaning table is arranged in the cleaning chamber, the chip is placed on the carrying table, the brush brushes the surface of the chip, the carrying table and the chip on the carrying table do not rotate when the rotation speed of the carrying table is zero, the brush brushes the surface of the chip in a fan-shaped swinging mode for 1-80 seconds, such as 1 second, 5 seconds, 10 seconds, 20 seconds, 30 seconds, 40 seconds, 50 seconds, 60 seconds, 70 seconds, 80 seconds or any two of the two components, the carrying table rotates the chip on the carrying table when the rotation speed of the carrying table is not zero, the rotation speed of the carrying table is 0-500RPM, such as 0, 20RPM, 50RPM, 100RPM, 150RPM, 200RPM, 300RPM, 400RPM, 500RPM or a range consisting of any two of the two, RPM means rotation times of each minute, such as 150RPM means 150RPM, namely the carrying table rotates 150RPM per minute, and the rotation speed of the carrying table is equal to the rotation speed of the chip. The chip automatic washer may be a conventional chip automatic washer, for example, a chip automatic washer of model C1502 BS.
Specifically, two-fluid cleaning devices are adopted to carry out two-fluid cleaning treatment, each two-fluid cleaning device comprises a two-fluid spray head, an air inlet pipe, a liquid inlet pipe and a connecting pipe, the liquid inlet pipe is connected with the two-fluid spray head through the connecting pipe, and the air inlet pipe is connected with the two-fluid spray head through the connecting pipe. In the two-fluid cleaning process, gas is introduced into the gas inlet pipe, liquid is introduced into the liquid inlet pipe, the gas is introduced into the two-fluid spray head through the connecting pipe by the gas inlet pipe, the liquid is introduced into the two-fluid spray head through the connecting pipe by the liquid inlet pipe, the gas in the gas inlet pipe and the liquid in the liquid inlet pipe are mixed in the connecting pipe to form two-fluid water-gas mixed liquid, the two-fluid water-gas mixed liquid generates two-fluid spray through the two-fluid spray head, the two-fluid spray washes the chip, the two-fluid spray enters into the pores on the surface of the chip, the moisture on the surface of the chip is blown off by utilizing the force of the gas, the cleaning effect is improved, and the cleaning treatment of the chip by the two-fluid spray is realized, wherein the gas comprises nitrogen.
In some embodiments, the time for the purge process with the two fluids is in the range of 1-600 seconds, such as 1 second, 15 seconds, 25 seconds, 35 seconds, 45 seconds, 60 seconds, 100 seconds, 200 seconds, 300 seconds, 400 seconds, 500 seconds, 600 seconds, or any two of these.
In some embodiments, a chip automatic cleaning machine is used for cleaning, the chip automatic cleaning machine comprises a cleaning table and a first nozzle, the chip is placed on the cleaning table, the nozzle is used for spraying two fluids on the cleaning table, the rotating speed of the cleaning table is 10-1500RPM (for example, 10RPM, 50RPM, 100RPM, 500RPM, 1000RPM, 1500RPM or a range formed by any two of the two fluids in the cleaning process, the two fluids comprise gas and liquid, the pressure of the liquid is 0.1-0.8MPa (for example, 0.1MPa, 0.12MPa, 0.2MPa, 0.4MPa, 0.5MPa, 0.6MPa, 0.7MPa, 0.8MPa or a range formed by any two of the two fluids), and the flow rate of the liquid is 0.1-0.8L/min (for example, 0.1L/min, 0.12L/min, 0.13L/min, 0.2L/min, 0.4L/min, 0.6L/min, 0.8L/min or a range formed by any two of the two fluids). For example, in some embodiments, the liquid in the two fluids is water, and the water pressure of the water may be controlled to be 0.1-0.8MPa during the cleaning process using the two fluids.
Specifically, the automatic chip cleaning machine comprises a cleaning chamber, a cleaning table arranged in the cleaning chamber, a first nozzle used for spraying first mixed liquid into the cleaning chamber of the cleaning machine, a second nozzle used for spraying second mixed liquid into the cleaning chamber of the cleaning machine, and a two-fluid nozzle used for spraying two fluids into the cleaning chamber of the cleaning machine. When the chip automatic cleaning machine is used for cleaning chips, the chips are placed on a cleaning table, the first mixed liquid is sprayed to the chips on the cleaning table through a first nozzle, the second mixed liquid is sprayed to the chips on the cleaning table through a second nozzle, and the two fluids are sprayed to the chips on the cleaning table through a two-fluid nozzle. Specifically, during the cleaning process using two fluids, the chip is placed on the cleaning table and rotated with the cleaning table, and the rotational speed of the chip is substantially equal to the rotational speed of the cleaning table.
In some embodiments, the drying is performed with compressed gas, which is compressed air, such as compressed nitrogen, at a pressure of 0.08-0.9MPa, such as 0.08MPa, 0.1MPa, 0.2MPa, 0.4MPa, 0.6MPa, 0.8MPa, 0.9MPa, or a range of any two thereof, for a drying time of 1-600 seconds, such as 1 second, 20 seconds, 30 seconds, 40 seconds, 80 seconds, 120 seconds, 200 seconds, 400 seconds, 600 seconds, or a range of any two thereof, and a control chip rotational speed of 100-2500RPM, such as 100RPM, 150RPM, 200RPM, 500RPM, 1000RPM, 1500RPM, 1800RPM, 2000RPM, 2500RPM, or a range of any two thereof.
Specifically, the chip automatic cleaning machine is adopted for drying treatment, the chip automatic cleaning machine comprises a cleaning chamber, a cleaning table arranged in the cleaning chamber, and a third nozzle for spraying compressed air into the cleaning chamber of the cleaning machine, and the specific process comprises the following steps: the chip is placed on the cleaning table, the rotation speed of the chip is basically equal to that of the cleaning table, compressed gas is sprayed towards the chip through the third nozzle to carry out drying treatment, the water remained on the chip is blown off by the force of the compressed air, the water on the chip is removed by the centrifugal force of the carrier table, and therefore drying is achieved.
In general, after the chip is cleaned by adopting the chip cleaning method, release paper can be attached to the surface of the cleaned chip, so that the cleaned chip is protected from being polluted, and the cleaned chip is more convenient to store.
The present invention will be further illustrated by the following specific examples and comparative examples.
Example 1
Chip cleaning is carried out on a chip automatic cleaning machine with the model of C1502BS, wherein the chip automatic cleaning machine comprises a cleaning chamber, a cleaning table (or a carrying table), a first nozzle for spraying first mixed liquid into the cleaning chamber of the cleaning machine, a second nozzle for spraying second mixed liquid into the cleaning chamber of the cleaning machine, a two-fluid nozzle for spraying two fluids into the cleaning chamber of the cleaning machine, and a third nozzle for spraying compressed gas into the cleaning chamber of the cleaning machine, wherein the chips are sorted LED chips, the carrier is a blue film, and the cold degreasing agent is a cold degreasing agent with the model of LF-106 of Dragon-Fei environmental protection technology Co., ltd, and the chip cleaning is carried out by adopting the following steps:
s1, placing the chip into an oven for first baking treatment, wherein the temperature of the oven is 35 ℃, and the baking time is 1200 seconds;
s2, placing the chip on a carrier, after spraying the first mixed liquid towards the chip for 12 seconds, immersing the chip, and after soaking for 5 seconds, brushing the surface of the chip for 30 seconds by using a brush in a fan-shaped swing mode, wherein the volume ratio of the cold degreasing agent to the deionized water in the first mixed liquid is: deionized water = 1:5, rotational speed of the carrier is 150RPM;
s3, washing the chip by adopting two fluids, wherein the rotating speed of the carrier is 1000RPM, the washing time is 35 seconds, the two fluids are nitrogen and water, the water pressure of the two fluids is 0.12Mpa, and the water flow is 0.13L/min;
s4, placing the chip on a weighing carrier, after spraying the second mixed solution towards the chip for 15 seconds, immersing the chip, and after soaking for 8 seconds, brushing the surface of the chip for 30 seconds by using a brush in a fan-shaped swing mode, wherein the volume ratio of cold degreasing agent to deionized water in the second mixed solution is that: deionized water = 1:12, rotational speed of the carrier is 150RPM;
s5, flushing the chip by adopting two fluids, wherein the rotating speed of the carrier is 1000RPM, the flushing time is 45 seconds, the two fluids are nitrogen and water, the water pressure of the two fluids is 0.1Mpa, and the water flow is 0.12L/Min;
s6, drying the surface of the chip by adopting compressed gas, wherein the pressure of the compressed gas is 0.1Mpa, the rotating speed of the carrier is 1800RPM, and the drying time is 40 seconds;
and S7, placing the chip into an oven for a second baking treatment to obtain a cleaned chip, and marking the cleaned chip as a sample 1, wherein the temperature of the oven is 45 ℃, and the baking time is 1500 seconds.
Example 2
The difference from example 1 is that in step S2, the volume ratio of cold degreasing agent and deionized water in the first mixed solution is: deionized water = 1:5 replacement with cold degreasing agent: deionized water=1:7, the rest of the conditions were the same as in example 1.
Example 3
The difference from example 1 is that in step S1, the oven temperature was 35 ℃, the baking time was 1200 seconds, the oven temperature was 40 ℃, the baking time was 900 seconds, and the other conditions were the same as in example 1.
Comparative example 1
The difference from example 1 is that step S1 is eliminated, and the other conditions are the same as in example 1.
Comparative example 2
The difference from example 1 is that the S4 step and S5 step are eliminated, and the other conditions are the same as in example 1.
Fig. 1 is a flowchart of a method for cleaning a chip according to an embodiment of the invention.
Fig. 2 is an overall appearance diagram of the cleaned chips in example 1, and it can be seen from fig. 2 that the chips obtained by the method for cleaning chips provided by the invention are orderly arranged, and the chips are complete and have no loss due to falling.
Fig. 3 is an EDS elemental analysis chart of an electrode region of a cleaned chip in example 2, and table 1 is an element composition table of an electrode region of a cleaned chip calculated from fig. 3, and it is understood from table 1 that the electrode region of a cleaned chip is mainly gold (Au) element on the surface of the electrode, except for trace amounts of carbon (C) and oxygen (O), indicating that the surface of the chip is cleaned and no residue is present.
Fig. 4 is an overall appearance of the chip after cleaning in comparative example 1, and as can be seen from fig. 4, the core particles were dropped during cleaning, which indicates that the adhesion between the core particles and the blue film was poor, and the core particles were lost during subsequent cleaning.
FIG. 5 is an EDS elemental analysis chart of the electrode area of the cleaned chip in comparative example 2, and Table 2 is a table of elemental composition of the electrode area of the cleaned chip calculated from FIG. 5. As can be seen from FIGS. 5 and 2, an increase in the content of C, O and other elements is detected in the electrode area of the chip, indicating an increase in organic lipid contaminants on the chip, and the lack of the second mixed liquor cleaning treatment, such that the cold degreasing agent is not completely dissolved and removed; in addition, other trace elements, such as aluminum (Al), chlorine (Cl), titanium (Ti), silver (Ag), etc., were detected in the electrode region of the chip, indicating that the chip cleaning effect was not good.
TABLE 1
TABLE 2
In summary, the chip cleaning method provided by the invention not only can effectively remove the metal, dust and other particle pollutants and grease pollutants on the surface of the chip and ensure that the surface of the chip has no secondary pollutants such as cleaning agent and the like, but also can ensure that the core particles do not fall off and ensure the integrity and quality of the chip, and in addition, the cleaning method is simple and convenient to operate and is especially suitable for batch cleaning of LED chips.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A chip cleaning method is characterized in that: the method comprises the following steps:
after the chip is subjected to the first baking treatment, cleaning the chip by adopting the first mixed liquid, the second mixed liquid and the two fluids in sequence, and drying the cleaned chip and then carrying out the second baking treatment; the first mixed liquid comprises a cold degreasing agent and water, and the second mixed liquid comprises a cold degreasing agent and water, wherein the volume concentration of the cold degreasing agent in the second mixed liquid is lower than that of the cold degreasing agent in the first mixed liquid;
the cold degreasing agent comprises at least one of LF-106 cold degreasing agent and HWJ-109 cold degreasing agent;
after the first mixed solution is adopted for cleaning treatment, the second fluid is adopted for cleaning treatment, and then the second mixed solution is adopted for cleaning treatment;
the cleaning treatment process by adopting the first mixed solution comprises the following steps: after the chip is soaked in the first mixed solution for 5-80 seconds, brushing the chip; and/or the number of the groups of groups,
the process of adopting the second mixed solution for cleaning treatment comprises the following steps: and (3) soaking the chip in the second mixed solution for 5-80 seconds, and then brushing the chip.
2. The method for cleaning a chip according to claim 1, wherein: the conditions of the first baking treatment are as follows: the baking temperature is 25-65 ℃, and the baking time is 300-1800 seconds; and/or the number of the groups of groups,
the conditions of the second baking treatment are as follows: the baking temperature is 25-65 ℃, and the baking time is 200-1800 seconds.
3. The method for cleaning a chip according to claim 1, wherein: in the first mixed solution, the volume ratio of the cold degreasing agent to the water is 1:1-1:15; and/or the number of the groups of groups,
the volume ratio of the cold degreasing agent to the water in the second mixed solution is 1:5-1:25.
4. The method for cleaning a chip according to claim 1, wherein: the chip automatic cleaning machine is adopted to carry out the brushing treatment, the chip automatic cleaning machine comprises a cleaning table and a brush used for the brushing treatment, the chip is placed on the cleaning table and is brushed by the brush in the brushing treatment process, the rotating speed of the cleaning table is 0-500RPM, and the brushing treatment time is 1-80 seconds.
5. The method for cleaning a chip according to claim 1, wherein: the two fluids include a gas and a liquid; and/or the time for the cleaning treatment with the two fluids is 1-600 seconds.
6. The method for cleaning a chip according to claim 1, wherein: the chip automatic cleaning machine is adopted to carry out the cleaning treatment, the chip automatic cleaning machine comprises a cleaning table and a first nozzle, the chip is arranged on the cleaning table, the nozzle is used for spraying two fluids on the cleaning table, the rotating speed of the cleaning table is 10-1500RPM in the cleaning treatment process by adopting the two fluids, the two fluids comprise gas and liquid, the pressure of the liquid is 0.1-0.8MPa, and the flow rate of the liquid is 0.1-0.8L/min.
7. The method for cleaning a chip according to claim 1, wherein: and (3) drying by adopting compressed gas, wherein the pressure of the compressed gas is 0.08-0.9MPa, the drying time is 1-600 seconds, and the rotating speed of the chip is controlled to be 100-2500RPM.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003031532A (en) * | 2001-07-18 | 2003-01-31 | Sony Corp | Semiconductor device manufacturing method and apparatus |
| CN102560488A (en) * | 2012-02-02 | 2012-07-11 | 天津大学 | DBC (Direct Bonded Copper) substrate surface treatment process based on nano-silver soldering paste connecting chip |
| CN112133796A (en) * | 2019-06-25 | 2020-12-25 | 山东浪潮华光光电子股份有限公司 | Method for improving surface cleanliness of LED tube core |
Family Cites Families (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100253583B1 (en) * | 1997-04-21 | 2000-04-15 | 김영환 | Fabricating method for junction soi wafer |
| US20040216770A1 (en) * | 2003-04-29 | 2004-11-04 | Taiwan Semiconductor Manufacturing Co., Ltd. | Process for rinsing and drying substrates |
| JP4435610B2 (en) * | 2004-03-23 | 2010-03-24 | パナソニック株式会社 | Dummy board |
| JP4613744B2 (en) * | 2005-08-10 | 2011-01-19 | 株式会社Ｓｕｍｃｏ | Cleaning method of silicon wafer |
| KR20070018689A (en) * | 2005-08-10 | 2007-02-14 | 가부시키가이샤 섬코 | Silicon wafer cleaning method |
| KR20100080162A (en) * | 2008-12-31 | 2010-07-08 | 주식회사 동부하이텍 | Chemical mechanical polishing device and chemical mechanical polishing method |
| JP2013106026A (en) * | 2011-11-14 | 2013-05-30 | Mac Sangyo Kiki Kk | Separation device and method of semiconductor wafer |
| JP5632860B2 (en) * | 2012-01-05 | 2014-11-26 | 東京エレクトロン株式会社 | Substrate cleaning method, substrate cleaning apparatus, and substrate cleaning storage medium |
| JP6023010B2 (en) * | 2013-06-26 | 2016-11-09 | 東京エレクトロン株式会社 | Substrate processing method, program, computer storage medium, and substrate processing system |
| JP6086059B2 (en) * | 2013-12-20 | 2017-03-01 | 信越半導体株式会社 | Wafer drying apparatus and wafer drying method |
| CN104037068B (en) * | 2014-07-09 | 2016-08-24 | 中国科学院半导体研究所 | A kind of method that chip surface dirt cleaning processes |
| CN206194778U (en) * | 2016-11-18 | 2017-05-24 | 济宁学院 | Emitting diode automation of welding belt cleaning device |
| CN107068820B (en) * | 2017-05-31 | 2019-03-01 | 山东浪潮华光光电子股份有限公司 | A method of improve in GaAs base LED chip cutting process and falls tube core |
| CN108330031A (en) * | 2017-12-19 | 2018-07-27 | 东莞市讯易机电科技有限公司 | A kind of cleaning method of silicon chip using special cleaning |
| CN111063609A (en) * | 2019-12-18 | 2020-04-24 | 武汉百臻半导体科技有限公司 | Semiconductor chip cleaning method |
| CN111162155B (en) * | 2020-01-03 | 2021-07-06 | 深圳市奥伦德元器件有限公司 | Power improving method for infrared LED chip made of gallium-aluminum-arsenic material |
| CN111048405A (en) * | 2020-01-07 | 2020-04-21 | 厦门英惟达智能科技有限公司 | Product cleaning process for digitally cleaning chip wafer |
| CN111375595A (en) * | 2020-03-31 | 2020-07-07 | 上海邦先医疗科技有限公司 | Biochip washs drying device |
| CN112354963A (en) * | 2020-10-13 | 2021-02-12 | 南通锐深环保科技有限公司 | Structured packing degreasing process |
| CN112420563A (en) * | 2020-11-30 | 2021-02-26 | 杭州醉夕风科技有限公司 | Chip recovery processing system |
-
2021
- 2021-07-21 CN CN202110827556.8A patent/CN113555274B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003031532A (en) * | 2001-07-18 | 2003-01-31 | Sony Corp | Semiconductor device manufacturing method and apparatus |
| CN102560488A (en) * | 2012-02-02 | 2012-07-11 | 天津大学 | DBC (Direct Bonded Copper) substrate surface treatment process based on nano-silver soldering paste connecting chip |
| CN112133796A (en) * | 2019-06-25 | 2020-12-25 | 山东浪潮华光光电子股份有限公司 | Method for improving surface cleanliness of LED tube core |
Non-Patent Citations (1)
| Title |
|---|
| 基于原子扩散的蓝宝石芯片键合技术研究;吴亚林;王世宁;曹永海;王伟;史鑫;;中国电子科学研究院学报(第02期);全文 * |
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