KR102486315B1 - Method Of Manufacturing Eco-Friendly High-Density Wiper For Semiconductor Clean Room - Google Patents

Abstract

The present invention relates to a method for manufacturing an eco-friendly high-density wiper for a semiconductor manufacturing clean room using a high shrinkage process without using a benzyl alcohol emulsion. And since the benzyl alcohol-based emulsion is not used during the high shrinkage process, NVR is reduced, which is eco-friendly, and energy / water is reduced by about 50% and manufacturing cost is reduced by about 25% or more. can

Description

Manufacturing method of eco-friendly high-density wiper for semiconductor manufacturing clean room {Method Of Manufacturing Eco-Friendly High-Density Wiper For Semiconductor Clean Room}

The present invention solves problems and environmental problems in semiconductor manufacturing due to non-volatile residue (NVR) by performing a high shrinkage process without using benzyl alcohol emulsion used in the high shrinkage process of microfiber wiper products used in the semiconductor manufacturing line. It relates to a method of manufacturing an eco-friendly high-density wiper for a semiconductor manufacturing clean room that can be solved.

Korea has the first and second largest companies in the global memory semiconductor market, and the combined market share of the two companies stands out in the global market with 73% of DRAM and 46% of NAND flash as of 2018.

As miniaturization of the semiconductor manufacturing process is accelerated, the possibility of defects occurring even with a small amount of impurities increases, so the importance of cleaning tends to increase. Cleaning is a very important process that accounts for about 15% of the main semiconductor processes and is directly related to product performance, reliability, and yield. When the circuit line width is miniaturized, the line becomes narrow and deep, making it more difficult to remove impurities, and the importance of cleaning is gradually increasing. It's growing.

Microfiber wiper products are a key product that directly affects the quality of semiconductors as a material used to clean them from contaminants such as various residues and foreign substances generated in the semiconductor manufacturing process.

Microfibers produced by composite spinning of two-component polymers have an excellent decontamination mechanism even in micro-curved areas that are difficult to remove due to a dramatic increase in surface area after the composite process. A high-shrinkage processing process using an alcohol emulsion and a high-performance wiper material using the same have been developed and used.

After Japan's Kanebo launched Verima X, a composite split yarn in 1975, KB Siren began to develop and commercialize Savina MX, a product for clean rooms. Industrial high-clean wipers are manufactured and widely used. Products produced by KB Siren are used as the best high-performance wipers in processes such as semiconductor/integrated circuit manufacturing or precision parts assembly for cameras.

These high-performance wiper products have been manufactured through high-shrinkage processing in which pre-treatment is followed by immersion/moist heat treatment in high-concentration NaOH aqueous solution to reduce division, and then high-shrinkage processing through batch or continuous benzyl alcohol emulsion treatment. It has excellent wiping properties compared to low-cost wipers, but as described above, it uses a high shrinkage process using benzyl alcohol, so it shows a relatively high NVR, so special attention is required for safe handling during the manufacturing process. In particular, these high-shrinkage, high-density wipers have a very dense structure once they are shrunk, so in order to discharge residual substances inside, they must be washed repeatedly under very harsh conditions, and it is difficult to completely remove them, making them more efficient than general wipers. A lot of non-volatile residues (NVR, Non-Volatile Residue) are being detected.

The NVR is recognized as a key performance because the chemicals used during the wiper manufacturing process are not completely removed and can contaminate the semiconductor during wiping. Such benzyl alcohol is mainly used as a preservative, but special care is required in handling it as a harmful substance known to cause allergies and have a risk of toxicity to internal organs (concern for infertility). In addition, as environmental regulations are increasingly being strengthened worldwide and eco-friendly processes are being emphasized, the application of eco-friendly manufacturing processes is urgently required.

Republic of Korea Patent Publication No. 10-2010-0032002 (published on March 25, 2010)

Therefore, in the present invention, in manufacturing a high-density wiper applicable to a semiconductor manufacturing process, which is a clean environment with extremely small particles, the generation of non-volatile residue (NVR) is minimized and an eco-friendly high-density wiper for a semiconductor manufacturing clean room that does not use a harmful process It is a technical task to provide a manufacturing method.

Therefore, according to the present invention, the DTY yarn of NP split composite yarn composed of a polyamide part and a polyester part is supplied to a double-sided circular knitting machine and knitted, then refined at 80 to 90 ° C, 100 to 130 ° C, under an alkaline solution, weight loss division and After high shrinkage processing, there is provided a method for manufacturing an eco-friendly high-density wiper for a semiconductor manufacturing clean room, characterized in that heat setting at 180 ~ 195 ℃, 30 ~ 40m / min.

Hereinafter, the present invention will be described in more detail.

The present invention solves problems and environmental problems in semiconductor manufacturing due to non-volatile residue (NVR) by performing a high shrinkage process without using benzyl alcohol emulsion used in the high shrinkage process of microfiber wiper products used in the semiconductor manufacturing line. It relates to a method of manufacturing an eco-friendly high-density wiper for a semiconductor manufacturing clean room that can be solved.

The manufacturing method of the eco-friendly high-density wiper for the semiconductor manufacturing clean room of the present invention is largely composed of DTY processing of yarn, knitting, scouring, weight loss division and high shrinkage processing in the order.

The yarn used in the present invention is an NP split composite yarn composed of a polyamide part and a polyester part, and TPA and IPA (Isophthalic acid) having a weight ratio of 80:20 to 90:10 in the polyester part react with EG (Ethylene Glycol) NP split composite yarn, which is made of high shrinkage polyester, is used.

General polyester is a condensation polymer of TPA (Terephthalic acid) and EG (Ethylene Glycol), and it is known that TPA mainly contributes to the formation of a crystalline region and EG contributes to the formation of an amorphous region. In the present invention, in the polymerization process, TPA and IPA (isophthalic acid) are supplied at a weight ratio of 80:20 to 90:10 and reacted with EG to copolymerize. become an ester.

NP-split composite yarn is produced by composite spinning of these high-shrinkage polyester and nylon resin in a conventional way. This high-shrinkage NP composite split yarn has a very high density through shrinkage processing, so it has dimensional stability and the specific surface area of the divided yarn is reduced. It has excellent wiping properties due to the increase.

The high-shrinkage NP composite split yarn thus prepared has the advantage of being able to achieve high shrinkage without using a benzyl alcohol-based emulsion through improved heat shrinkability by adding IPA in the polymerization process to increase the amorphous region of the polyester part.

In the present invention, rather than using the NP composite divided yarn as it is, twist and untwist while applying heat to the NP composite divided yarn to impart bulkiness to the filament yarn and at the same time to promote initial division at the NP interface DTY processed yarn It is made and used for weaving or knitting.

This DTY processed yarn passes the NP split composite yarn through the first feed roller, heat-treats it in the first heater at 140 to 160 ° C, and then passes through the second feed roller while combusting at a combustible ratio of 1.3 to 1.4 with a disk-type twisting device. After stretching at a draw ratio of 1.10 to 1.35, interlaced with an air pressure of 13 to 16 kgf/cm2, and then wound at a thread speed of 400 to 550 m/min.

When the temperature of the first heater is less than 140° C., the bulkiness of false-twisted yarn is deteriorated, and when it exceeds 160° C., unstretched yarn or fusion may occur.

After the false twisting, the second feed roller is passed through, and the filament is drawn by using the speed difference between the first feed roller and the second feed roller. At this time, it is preferable that the draw ratio is 1.10 to 1.35 times. If the draw ratio is less than 1.10 times, non-twisting occurs and the uniformity of false twist yarns deteriorates. cause problems with

After the stretching, the interlace nozzle is entangled and wound with a take-up roller at a thread speed of 400 to 550 m/min to complete the DTY processing work. The filaments passing through the second feed roller are entangled to improve convergence. The pressure is preferably 13 to 16 kgf/cm2. If the pressure exceeds 16 kgf/cm2, interlaced marks may occur on the surface of the fabric after knitting. can

The DTY processing yarn of the NP split composite yarn prepared in this way is supplied to the double-sided circular knitting machine and knitted.

After the above knitting, scouring at 80 ~ 90 ℃, 100 ~ 130 ℃, weight loss division and high shrinkage processing under an alkali solution, followed by heat setting at 180 ~ 195 ℃, 30 ~ 40 m / min Eco-friendly high-density wiper for clean room of the present invention will manufacture

The refining process is performed at 80 to 90 ° C for 15 to 20 minutes, and the weight loss division process and high shrinkage process are performed at 100 to 130 ° C under an alkali (NaOH) solution. Heat setting is 180 ~ 195 ℃, 30 ~ 40m / min and stays in the heat setting chamber for 50 ~ 60 seconds.

In the case of the splitting and high shrinkage processing, it is preferable that the degree of splitting is 80 to 90% and the shrinkage ratio is 20 to 30% for the shape stability and wiping property of the high-density wiper.

The high-shrinkage processing of microfiber wipers using existing NP split yarns used benzyl alcohol-based emulsion for structural transformation of the polymer chain of synthetic fibers, but the benzyl alcohol is known to have toxicity to internal organs, requiring caution in handling and wastewater It has a fatal disadvantage that is difficult to process, so conversion to an environmentally friendly process is urgently required.

In addition, the existing microfiber wipers using NP split yarns have excellent wiping properties compared to general low-priced wipers, but show relatively high NVRs because they are applied with a high shrinkage process using benzyl alcohol as described above. These high-shrinkage, high-density wipers have a very dense structure once they are shrunk, so in order to discharge residual substances inside, they must be washed repeatedly under very harsh conditions. is produced by adding IPA in the polymerization process to increase the amorphous region of the polyester part, so that high shrinkage is possible without using benzyl alcohol-based emulsion through improved heat shrinkage, so NVR can be greatly reduced because little chemicals are used. It is very advantageous in terms of cost as it can simplify the water washing process.

Therefore, according to the present invention, the wiping performance is excellent, but the existing processes of weight loss division and high shrinkage are integrated, and the benzyl alcohol-based emulsion is not used during the high shrinkage process, so NVR is reduced and eco-friendly, and energy / water is about 50%, It is possible to provide a method of manufacturing an eco-friendly high-density wiper for a semiconductor manufacturing clean room capable of reducing manufacturing cost by about 25% or more.

1 is a surface micrograph of an eco-friendly high-density wiper for a semiconductor manufacturing clean room manufactured according to Example 1 of the present invention,
2 is a cross-sectional micrograph of an eco-friendly high-density wiper for a semiconductor manufacturing clean room manufactured according to Example 1 of the present invention.

In the following embodiment, there is a non-limiting example of manufacturing an eco-friendly high-density wiper for a semiconductor manufacturing clean room of the present invention.

[Example 1]

NP composite split yarn (75D/48f, 7 splits, PET:Nylon= 75D/48f, 7 splits, PET:Nylon= 70:30) was processed by DTY under the conditions of Table 1 below, and then supplied to a double-sided circular knitting machine and knitted with an interlock tissue (32G).

Refining was carried out at 90 ° C x 15 min, reduced division / high shrinkage (liquid flow rapid) at 130 ° C for 20 min, and NaOH 3.0% concentration, so that the division was 80% and the shrinkage was 20%. Heat setting conditions were performed under conditions of 185 ° C. x 40 m/min.

process factor control condition YS (Four Speed) 450m/min DR (Draw ratio) 1.12 Disc conf. (Disc specification) 1 - 6 - 1 (52 × 3T × 14.45) HT1 (heater temperature) 145℃ DS/YS (disk speed/dead speed) 1.40 OF1 (confounding OF) 4.5% OF2 (Wound OF) 5.5% T1 (twist tension) 25gf T2 (relaxation tension) 20gf T3 (winding tension) 3.5gf Air nozzle 1.4Φ air pressure 15kgf/cm²

[Comparative Example 1]

General NP split yarns on a double-sided circular knitting machine It is supplied and knitted with an interlock structure (32G), scouring at 90℃ x 15min, weight loss division at 100℃ for 30 minutes under a concentration of 3.0% NaOH, and then high shrinkage at 130℃ for 20min using a benzyl alcohol emulsion with a division degree of 80 %, and the shrinkage rate was 20%. Heat setting conditions were performed under conditions of 185 ° C. x 40 m/min.

The physical property analysis results of the wipers of Example 1 and Comparative Example 1 are shown in Table 2 below.

division unit Example 1 Comparative Example 1 Assessment Methods Shrinkage (width direction) % 20 20 KS K ISO 22198 Apparent density g/cm ³ 0.30 0.30 KS K 0642 8.3.2 split view % 80 80 microscopy
- Measure the number of divided yarns in the fabric state
- Check the results by testing in the presence of external experts RoHS - PASS - Quantitative analysis through GC, LC, ICP, etc.
- For heavy metals, use acid to make the material low-molecular and quantitatively analyze using a spectrometer.
-Compounds were extracted using an extractor and quantitatively analyzed using a spectrometer. REACH - PASS - NVR IPA g/m ² 0.013 0.427 Precisely measures the weight of one wiper to 5 significant digits.
After stirring in an orbital shaker with 100 ml of solvent
Put the stirring solution in a 250㎖ round flask equipped with a reflux condensor and concentrate the solvent to 10㎖ or less using a hot plate.
Pour this concentrate into a weighed Aluminum Dish.
Put it in a 200℃ oven, evaporate the solvent, and measure the weight. DIW g/m ² 0.001 0.001 absorption
hour horizontal sec 7 41 Imprint in the center of the specimen using a rubber stamp with a diameter of 6 cm.
After adding 1ml of water using an auto dispensor to the center from 1cm above the specimen, measure the time for the water to reach the engraved part vertical method sec 39 304 Cut the specimen into 2cm in width and 5cm in length and mark the line at 1cm and 4cm on the specimen.
A 0.5 cm section of the specimen is immersed in water and the time from the point of passage of 1 cm to the point of passage of 4 cm is measured. absorption amount ml/g 3.06 1.63 Weigh the wiper
Immerse the wiper in a water bath of DI water for 30 seconds.
Take out the wiper that has been absorbed and wipe it off naturally for 30 seconds.
After dehydrating water, measure the weight of the dehydrated specimen to two decimal places. Particle >0.5μm ea/㎡ 14x10 ⁶ 13x10 ⁶ Put 1 piece of wiper into the Sus Tray containing 100 ml of DI Water and stir for 3 minutes at 100 rpm using a Biaxial Shaker.
Measure and record the number of particles per ml using a liquid particle counter. Lint
(Fiber) >100μm ea/sh 24 53 1 piece of wiper is placed in a Sus Tray containing 100 ml of DI Water.
Add and stir for 3 minutes at 100 rpm using an orbital shaker.
After taking out the wiper with tweezers, the stirred DI water
Filtration using a filter equipped with filter paper.
After drying the filtered filter paper, use a microscope to record the number of lint over 100 microns. >300μm ea/sh 17 22

Claims (4)

The NP split composite yarn composed of the polyamide part and the high shrinkage polyester part formed by reacting TPA and IPA (Isophthalic acid) with EG (Ethylene Glycol) in a weight ratio of 80:20 to 90:10 is passed through the first feed roller and 140 After heat treatment in the 1st heater at ~ 160℃, it is stretched at a draw ratio of 1.10 to 1.35 while passing through the second feed roller while combusting at a burn rate of 1.3 to 1.4 with a disk type combustible device, and then stretched at an air pressure of 13 to 16 kgf/cm2. After entanglement, the DTY yarn wound at a yarn speed of 400 to 550 m/min is supplied to a double-sided circular knitting machine and knitted, then refined at 80 to 90 ° C, 100 to 130 ° C, After weight loss division and high shrinkage processing in an alkaline solution, A method of manufacturing an eco-friendly high-density wiper for a semiconductor manufacturing clean room, characterized in that heat-setting at 180 ~ 195 ℃, 30 ~ 40m / min. delete delete According to claim 1,
Method of manufacturing an eco-friendly high-density wiper for semiconductor manufacturing clean room, characterized in that the division degree is 80 to 90% and the shrinkage rate is 20 to 30% during weight loss division and high shrinkage under the alkali solution.

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