JP5292923B2 - Microorganism detection method, microorganism detection apparatus, and slurry supply apparatus using the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a microorganism detection method and a microorganism detection apparatus to detect the presence of microorganisms by discriminating microorganisms in a flowing liquid from solid materials other than microorganism. <P>SOLUTION: The microorganism detection apparatus is provided with a light-emission part 204 to radiate a sample liquid flowing in a pipe with light of the first wavelength, a light receiving part 205 to detect the transmission amount of the light of the first wavelength through microorganisms and the transmission amount of the light through the solid materials other than microorganism, a light-emission part (204) radiating the sample liquid with light of the second wavelength, a light-receiving part (205) to detect the transmission amount of the light of the second wavelength through the solid materials other than microorganism, and an operation part 206 to calculate the difference between the transmission amount of the light of the first wavelength through the microorganisms and the solid materials other than microorganism and the transmission amount of the light of the second wavelength through the solid materials other than microorganism, wherein the presence of microorganisms is detected by the transmission difference calculated by the operation means 206. <P>COPYRIGHT: (C)2010,JPO&amp;INPIT

Description

  The present invention relates to a microbe detection method, a microbe detection device, and a microbe detection device for detecting microbes by identifying solid particles other than microbial particles in a liquid to be measured in which microbial particles and solid particles other than microbial particles are mixed and flowing. The present invention relates to a slurry supply apparatus using the same.

  To a chemical-mechanical polishing (CMP) apparatus, particularly when performing planar processing of a semiconductor substrate surface in semiconductor manufacturing, using a liquid to be measured in which microbial particles and solid particles other than microbial particles are mixed and flowing. A slurry that is a mixed liquid of a plurality of polishing stock solutions to be supplied may be mentioned. 2. Description of the Related Art In recent years, a CMP method as a microfabrication technique for high integration and high performance of a semiconductor device includes a mixed polishing liquid (hereinafter referred to as a slurry) in which a plurality of polishing stock solutions having different components are mixed, and an object to be polished. Is a polishing method in which the chemical action between the two and the mechanical action of the abrasive grains are combined, and the planarization of the interlayer insulating film, the formation of the metal plug, the embedded metal wiring type in the semiconductor manufacturing apparatus process, particularly in the multilayer wiring forming process It is an indispensable process.

  As a polishing apparatus used in this CMP, a disk-shaped polishing surface plate having a polishing cloth affixed to the surface, and a plurality of wafers that hold one surface of the wafer to be polished and abut the other surface of the wafer against the polishing cloth A wafer holding head and a head driving mechanism for rotating the wafer holding head relative to the polishing surface plate are provided, and polishing is performed by supplying a slurry containing abrasive grains between the polishing cloth and the wafer.

  Slurries are usually abrasive dispersions (mechanical polishing components) such as metal oxides, chemical polishing components comprising an oxidizing agent such as hydrogen peroxide or an alkali such as KOH, a dispersion aid, a pH adjuster, a diluent, etc. Contains. In the CMP method, it is extremely important to maintain the accuracy of the mixing ratio and supply amount of a plurality of polishing stock solutions such as abrasive dispersions having different slurry components and hydrogen peroxide, and to prevent aggregation and sedimentation. In addition, in order to stabilize the polishing rate and improve the accuracy of flattening, the particle size or particle size distribution of the abrasive grains in the slurry supplied to the flattening step must be stable, and other impurities and foreign matters can be prevented from being mixed. Is also an important factor. As dispersion aids, organic substances such as surfactants and organic acids are often used. Here, the fact that the concentration of a chemical polishing component such as an oxidizing agent is stable is also an important factor for improving the flattening accuracy.

  Moreover, since the pH of the abrasive dispersion and slurry is neutral, the composition sufficiently allows the growth of aerobic microorganisms. Although the preparation of the slurry and the operation of supplying the slurry to the polishing apparatus are continuously performed, it is inevitable that aerobic microorganisms are present in the abrasive dispersion. For this reason, as time passes, microorganisms are formed on the inner wall of the abrasive dispersion supply line and the supply line to the polishing apparatus for the slurry after mixing a plurality of polishing stock solutions such as abrasive dispersions of different components and hydrogen peroxide. It has been confirmed that it adheres and propagates and partially becomes a lump. In particular, there is a tendency for aerobic microorganisms to locally adhere, multiply and agglomerate at the bent portions of the abrasive dispersion supply line and the slurry supply line. Further, when a resin material such as PFA (perfluoroalkyl copolymer) is used for the piping of each supply line, the above tendency becomes more prominent.

  As described above, when microorganisms adhere to the inner wall portion of the abrasive dispersion supply line and propagate and become partially agglomerated, the flow resistance of the abrasive dispersion supply line increases, This results in a decrease in the feed rate of the grain dispersion. Furthermore, the mixing ratio of the abrasive dispersion and the hydrogen peroxide solution varies, making it difficult to control to a predetermined component ratio.

  Furthermore, when a flow meter is used, the accuracy of flow rate measurement due to the adhesion of microorganisms decreases, and it becomes difficult to control the flow rate to a predetermined component ratio. In addition, when a mixer is used, microorganisms adhere to the mixing promoting member and the inner wall and propagate, and uniform mixing cannot be performed in the mixer. In addition, when microorganisms adhere to the inner wall of the slurry supply line and grow, the flow resistance increases with respect to the flow of the slurry, resulting in a decrease in the amount of slurry supplied to the polishing equipment, and the accuracy of the supply amount. Can't keep up.

  The adhesion and propagation of microorganisms in the abrasive dispersion supply line and the slurry supply line increase with the use time of the slurry supply apparatus, and there is a risk that the flow path may be blocked, particularly at the bent portion of the supply line. . For this reason, it becomes difficult to control to a predetermined mixing ratio and to make the supply amount of slurry to the polishing apparatus constant. In addition, if a part of the microbial mass is peeled off as small pieces or particles due to the adhesion or propagation of microorganisms, and this reaches the polishing machine as foreign matter, it will have a serious adverse effect on the polishing performance of the wafer. Become.

  In order to solve the above-mentioned problems caused by aerobic microorganisms, a bactericide is conventionally added to the abrasive dispersion, but it is in a situation where no aerobic microorganisms can be eliminated. For this reason, the following is known, in which a slurry supply device is provided with an abrasive dispersion supply line and a part of the slurry supply line provided with microbial contamination prevention means such as heating and cooling unit means.

  An apparatus for supplying a polishing fluid containing a CMP slurry material to a polishing apparatus, the first storage means storing a first polishing fluid, and the second storing a second polishing fluid. Storage means, means for mixing the first polishing fluid and the second polishing fluid, the first storage means, the second storage means, and the mixing means from any of these storage means Cooling of the polishing fluid, heating by microwave irradiation, provided in any part of the piping for feeding the polishing fluid to the means and the piping for feeding the polishing fluid obtained by mixing, It is provided with a means for preventing microbial contamination by irradiation of cytotoxic electromagnetic waves and / or sound waves (for example, Patent Document 1).

Also, a polishing liquid manufacturing apparatus that manages in-line the generation of abrasive grains having a predetermined particle size or more in the polishing liquid, a preparation tank for preparing a polishing liquid having a constant abrasive concentration, and circulating the prepared polishing liquid And a polishing liquid circulating device. In the bypass conduit with adjustable flow rate of the conduit of the polishing liquid circulating apparatus, the light blocking type polishing liquid monitoring particles for detecting and measuring the number of abrasive grains having a particle diameter equal to or larger than the predetermined particle diameter. A detector is provided (for example, Patent Document 2).
JP 2003-197576 A JP 2002-154056 A

  However, what is described in Patent Document 1 described above always drives the microbial contamination preventing means regardless of the presence or absence of microorganisms in the polishing fluid. For this reason, even if there are no microorganisms in the polishing fluid, the microorganism contamination prevention means is driven, and there is a problem in energy saving, and the presence or absence of microorganisms in the polishing fluid and the propagation of microorganisms It is impossible to continuously and quickly grasp and confirm the actual effects of driving trends and microbial contamination prevention means.

  Moreover, although what was described in above-mentioned patent document 2 can detect the abrasive grain more than the predetermined particle size which is the solid substance in the prepared polishing liquid, it detects the microorganisms which exist in polishing liquid. I can't. For this reason, the problem which cannot prevent the bad influence to the grinding | polishing apparatus by presence of the above microorganisms was had.

  The present invention solves the above-mentioned conventional problems, and provides a microorganism detection method and a microorganism detection apparatus capable of detecting the presence of microorganisms by discriminating between microorganisms in a flowing liquid and solids other than microorganisms. The purpose is to do.

In order to solve the above-described conventional problems, the microorganism detection method of the present invention irradiates light having first and second different wavelengths into a liquid to be measured containing abrasive grains and flowing , the light and UV, the light of the second wavelength is infrared, the transmission amount of the abrasive grains is a solid non-microbial and microbial by light in the first wavelength, other than microorganisms by light in the second wavelength The presence of microorganisms is detected based on the difference from the amount of permeation of the abrasive grains , which is a solid material .

Moreover, microorganism detection apparatus of the present invention, the test liquid flowing was tube body containing abrasive grains, a light emitting unit for emitting light of a first wavelength is ultraviolet light, before Symbol of the first wavelength light a light receiving portion for detecting a permeation amount of the abrasive grains is a solid non-permeation amount and microorganisms by microorganisms, wherein the target solution, a light emitting unit for emitting light of the second wavelength is an infrared, before Symbol first A light receiving unit that detects a transmission amount of the abrasive grains that are solids other than microorganisms of light having a wavelength of 2, and transmission of the abrasive grains that are solids other than microorganisms and microorganisms by irradiation with light of the first wavelength. And calculating means for calculating the difference between the amount and the transmission amount of the abrasive grains which are solids other than microorganisms by irradiation with light of the second wavelength, and the microorganisms by the difference in the transmission amount calculated by the calculating means It is characterized by detecting the presence of.

Further, slurry dispenser of the present invention, the microorganism according to the detecting any site microorganisms leading to the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock A detection device is provided.

Microorganism detection method of the present invention, according to the microorganism detection apparatus, by determining the abrasive is a solid other than microorganisms and microorganisms in a flowing liquid containing abrasive grains, to detect the presence of microorganisms it can.

1st invention irradiates light of the 1st and 2nd different wavelength in the to-be-measured liquid containing an abrasive grain, makes the light of the said 1st wavelength into an ultraviolet-ray, and makes light of the 2nd wavelength Infrared, the amount of transmission of the abrasive grains that are solids other than microorganisms and microorganisms by light at the first wavelength, and the amount of transmission of the abrasive grains that are solids other than microorganisms by light at the second wavelength The microorganism detection method is characterized in that the presence of microorganisms is detected based on the difference between the two.

Thus, by determining the abrasive is a solid other than microorganisms and microorganisms in a flowing liquid containing abrasive grains, it is possible to detect the presence of microorganisms. Abrasive grains that are solids other than microorganisms can be reliably identified.

The second invention, the test liquid flowing was tube body containing abrasive grains, a light emitting unit for emitting light of a first wavelength is ultraviolet light, the transmission amount of microorganisms before Symbol first wavelength light and a light receiving portion for detecting a permeation amount of the abrasive grains is a solid other than microorganisms, said the target solution, a light emitting unit for emitting light of the second wavelength is an infrared, before Symbol of the second wavelength A light receiving unit for detecting the transmission amount of the abrasive grains that are solids other than microorganisms of light; the transmission amount of the abrasive grains that are solids other than microorganisms and microorganisms by irradiation with light of the first wavelength; Computation means for computing a difference from the transmission amount of the abrasive grains, which are solids other than microorganisms, by irradiation with light of the second wavelength, and detecting the presence of microorganisms by the difference in the transmission amount calculated by the calculation means The present invention provides a microorganism detecting device characterized by

Thus, by determining the abrasive is a solid other than microorganisms and microorganisms in a flowing liquid containing abrasive grains, it is possible to detect the presence of microorganisms. Abrasive grains that are solids other than microorganisms can be reliably identified.

  According to a third aspect of the present invention, there is provided the microorganism detecting apparatus according to the second aspect, wherein the permeation amount is an integrated value in a predetermined amount of the liquid to be measured that flows.

  Thereby, even if there is a trace amount of microorganisms, it can be detected accurately.

  According to a fourth aspect of the present invention, there is provided the microorganism detecting apparatus according to the second or third aspect of the invention, wherein the transmission amount of the first wavelength light and the second wavelength light is measured with a spectrum analyzer. .

  As a result, the transmission amount of each light can be continuously and accurately measured.

According to a fifth invention, in any one of the second to fourth inventions, there is provided a microorganism detecting apparatus comprising an informing means for informing the presence of a microorganism.

  As a result, the presence of microorganisms in the liquid to be measured can always be grasped, and a prompt treatment corresponding to this can be performed.

The sixth aspect of the present invention, any one of claims 2-5 for detecting any site microorganisms leading to the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock 1 A slurry supply device comprising the microorganism detection device according to the item.

  Accordingly, when microorganisms are detected by the microorganism detection device, it is possible to quickly cope with the adverse effect on the polishing device. Therefore, it is possible to always maintain stable polishing in the polishing apparatus.

A seventh aspect of the sixth invention, the plurality of portions extending in the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock that, with a microorganism detection apparatus A slurry supply device characterized by the above.

Thus, in the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock, it is possible to identify the site or breeding sites presence of microorganisms.

An eighth aspect of the invention, microorganisms in the sixth invention, a plurality of portions extending in the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock, the grinding stock or slurry The slurry supply device is characterized by being led out by a detection device.

Thus, in the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock, to identify the site or breeding sites by reducing the number of microorganisms detection means for presence of microorganisms Can do.

A ninth aspect of the invention, as in one of the sixth to eighth, at least a portion of the part extending in the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock The slurry supply device comprises a sterilizing means for sterilizing microorganisms and drives the sterilizing means based on the detection of the number of microorganisms by the microorganism detecting device.

  Accordingly, it is possible to prevent the discharge of microorganisms to the polishing apparatus, to prevent a change in flow rate due to an increase in flow resistance in the polishing fluid supply path due to the propagation of microorganisms, and to stabilize the mixing ratio. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.

A tenth invention is, in any one of the sixth to ninth, at least part of the part extending in the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock A cleaning means for cleaning, and based on a detection value of the number of microorganisms by the microorganism detection device, at least a part from the supply line of the polishing stock solution to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing device A slurry supply apparatus is characterized in that the part is washed.

  Accordingly, it is possible to prevent a change in flow rate due to an increase in flow resistance in the polishing fluid supply path due to the propagation of microorganisms, and to stabilize the mixing ratio. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.

An eleventh invention, in the tenth aspect, at least a portion of the supply line leading to the polishing apparatus of the slurry is a mixed grinding stock prior Symbol Migaku Ken stock from the supply line of polishing stock solution, tetramethylammonium hydroxide (TMAH ) After supplying and discharging the liquid, the slurry supply device is characterized in that the hydrogen peroxide solution is supplied and discharged.

  As a result, the cells of the microorganisms that have adhered and propagated by the tetramethylammonium hydroxide (TMAH) solution are dissolved, and further, the removal of the microorganisms by the reaction between the TMAH solution and the hydrogen peroxide solution is promoted, and the cells are reliably removed and washed. be able to. Therefore, it is possible to prevent a change in flow rate due to an increase in flow resistance in the polishing fluid supply path due to the propagation of microorganisms, and to stabilize the mixing ratio. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.

A twelfth aspect of the invention is the slurry supply apparatus according to the eleventh aspect , wherein an aqueous tetramethylammonium hydroxide solution is supplied and retained in a supply line for a predetermined time.

  As a result, the tetramethylammonium hydroxide solution, which is an organic strong alkali substance, sufficiently contacts and penetrates the microorganisms that adhere to and propagate on the inner wall even at the bent part of the supply line and are partially agglomerated. In addition, microbial cells can be lysed and sterilized.

A thirteenth aspect of the invention is the slurry supply apparatus according to the eleventh or twelfth aspect of the invention, wherein hydrogen peroxide water is supplied and retained in the supply line for a predetermined time.

  As a result, the tetramethylammonium hydroxide solution, which is a strong alkaline substance that remains on the inner wall of the supply line, and the microorganisms react with the hydrogen peroxide solution to fire, and from the inner wall of the microorganisms dissolved by the tetramethylammonium hydroxide solution. It is possible to further promote peeling and sterilization of the inner wall of the supply line.

Example 1
Hereinafter, a microorganism detection method, a microorganism detection apparatus of the present invention, and a slurry supply apparatus of Example 1 using the same will be described with reference to FIGS. FIG. 1 is a basic configuration diagram of a slurry supply apparatus of the present invention, FIG. 2 is a basic configuration diagram of a microorganism detection device in FIG. 1, and FIG. 3 is an example of an output signal (light transmission amount) from a light receiving unit of the microorganism detection device. FIG. 4 is a configuration diagram of the slurry supply apparatus showing a state of the first step during cleaning to discharge the abrasive dispersion by supplying pure water, and FIG. 5 is a state of the second step during cleaning supplying the TMAH solution. FIG. 6 is a configuration diagram of the slurry supply apparatus showing the state of the third step during cleaning for discharging the TMAH liquid by supplying nitrogen gas, and FIG. 7 is at the time of cleaning supplying hydrogen peroxide water. FIG. 8 is a configuration diagram of the slurry supply apparatus showing the state of the fifth step at the time of cleaning to discharge the hydrogen peroxide solution by pure water supply, and FIG. 9 is nitrogen. Drain pure water from gas supply It is a configuration diagram of a slurry dispenser showing the state of the sixth step of Kiyoshiji. FIG. 10 is a basic configuration diagram of another slurry supply apparatus of the present invention.

  In FIG. 1, first, the basic configuration of the slurry supply apparatus will be described. A predetermined amount of polishing stock solution 2 is stored in the abrasive dispersion container 1, and nitrogen gas is dispersed from the nitrogen gas supply line 3 through the on-off valve 4 in the abrasive dispersion container 1. Pressurize the upper surface of the liquid 2. An abrasive dispersion supply pipe 6 is provided in the abrasive dispersion container 1 and communicates with the abrasive dispersion supply line 7. The nitrogen gas supply line 3 and the abrasive dispersion liquid supply line 7 are fixed to the detachable member 5 and configured to be detachable from the abrasive dispersion container 1. The abrasive dispersion 2 is a slurry stock solution for slurry containing fine abrasive particles such as silica, ceria, alumina, zirconia, and manganese dioxide. The abrasive dispersion supply pipe 6 may be configured integrally with the abrasive dispersion supply line 7.

  The abrasive dispersion 2 is supplied to the mixed storage container 11 through the on-off valve 8 and the three-way switching valve 10 of the abrasive dispersion supply line 7. The abrasive dispersion supply line 7 is provided with a plurality of bent portions 9 in the mounted state. A slurry 12 which is a mixed polishing liquid of abrasive dispersion 2 and a hydrogen peroxide solution and pure water described later is stored in the mixed storage container 11.

A hydrogen peroxide solution (H ₂ O ₂ ) 14 as a polishing stock solution is stored in the hydrogen peroxide solution container 13, and nitrogen gas is supplied from the nitrogen gas supply line 15 through the opening / closing valve 16 into the hydrogen peroxide solution container 13. The upper surface of the hydrogen peroxide solution 14 is pressurized. A supply pipe 18 is provided in the hydrogen peroxide solution container 13 and communicates with a hydrogen peroxide solution supply line 19. Further, the nitrogen gas supply line 15 and the hydrogen peroxide solution supply line 19 are fixed to the detachable member 17 and configured to be detachable from the hydrogen peroxide solution container 13. The hydrogen peroxide solution 14 is supplied to the mixed storage container 11 through the open / close valve 20 of the hydrogen peroxide solution supply line 19.

  Pure water which is a polishing stock solution for dilution is supplied from the pure water supply line 21 to the mixed storage container 11 through the pure water branch line 22 and the open / close valve 23. A circulation line 24 is formed in the mixed storage container 11 to promote mixing in the mixed storage container 11 by driving a pump 25 and prevent sedimentation of abrasive grains.

  The slurry 12 is supplied from the mixed storage container 11 to the slurry mixed storage container 28 through the slurry supply line 26 and the on-off valve 27 by a drop pressure, and a predetermined amount of the slurry 29 is stored. A circulation line 30 is formed in the slurry mixing storage container 28, and the mixing is promoted in the slurry mixing storage container 28 by driving the pump 31, and the settling of abrasive grains is prevented. The slurry 29 is supplied to the polishing apparatuses 34 and 37 by driving the slurry supply lines 32 and 35 connected to the circulation line 30 and the pumps 33 and 36.

  A predetermined amount of tetramethylammonium hydroxide liquid 39 (hereinafter referred to as a TMAH liquid) is stored in a TMAH liquid container 38, and a TMAH liquid supply line 40 opened in the TMAH liquid container 38 is provided with a three-way switching valve. 41, an on-off valve 42, a three-way switching valve 43, and a cleaning liquid supply line 44 are connected to the three-way switching valve 10. The TMAH solution 39 is an organic strong alkali substance, and is prepared by diluting a TMAH stock solution to a concentration of 25 percent with ultrapure water.

  Nitrogen gas is pressurized from the nitrogen gas supply line 45 through the on-off valve 46 to pressurize the upper surface of the TMAH liquid 39 in the TMAH liquid container 38. A branch line 47 branched from the nitrogen gas supply line 45 is connected to the TMAH liquid supply line 40 via an on-off valve 48.

  A predetermined amount of hydrogen peroxide solution 50 is stored in the hydrogen peroxide solution container 49, and a hydrogen peroxide solution supply line 51 opened in the hydrogen peroxide solution container 49 is connected to the three-way switching valve 41. Nitrogen gas is pressurized from the nitrogen gas supply line 52 through the on-off valve 53 to pressurize the upper surface of the hydrogen peroxide solution 50 in the hydrogen peroxide solution container 49. A branch line 54 branched from the nitrogen gas supply line 52 is connected to a hydrogen peroxide solution supply line 51 via an on-off valve 55.

  A branch line 56 branched from the pure water supply line 21 connects pure water to the three-way switching valve 10 via an on-off valve 57.

  Further, in the basic configuration of FIG. 1, each of the abrasive dispersion supply line 7 and the circulation lines 24 and 30 is provided with a microorganism detecting device 200 and a sterilizing means 300 located on the downstream side of the microorganism detecting device 200. Out.

  2 (a) and 2 (b) show the basic configuration of the microorganism detection apparatus 200, FIG. 2 (a) is a partial cross-sectional configuration diagram of the microorganism detection apparatus 200, and FIG. 2 (b) is a diagram of FIG. 2 (a). It is sectional drawing in the AA line. The connecting member 202 is provided at both ends of the tubular body 201 made of transparent quartz glass or the like that transmits light, and the pipe 201a has a rectangular cross section, and the detection line 203 is connected to both ends of the connecting member 202. . A light emitting unit 204 is provided on one side of the tube body 201, and a light receiving unit 205 is provided on the other side facing the light emitting unit 204 across the tube body 201. Each of the microorganism detection devices 200 is located in a bypass flow path constituted by a detection line 203 branched from each of the abrasive dispersion supply line 7 and the circulation lines 24 and 30.

  The light emitting unit 204 has an ultraviolet light source and an infrared light source (not shown), and the tube 201 and the light receiving unit 205 receive light of different wavelengths including the first wavelength ultraviolet light and the second wavelength infrared light. Irradiate toward. The ultraviolet light and infrared light are irradiated by forming a flat belt-like light beam having a predetermined width in the tube length direction of the tube body 201 by a condenser lens (not shown). Moreover, it has comprised so that it can irradiate the whole pipe line 201a. As the ultraviolet light source included in the light emitting unit 204, for example, a mercury lamp that emits ultraviolet light having a wavelength of about 253.7 nm, which allows the microorganism to absorb ultraviolet energy well, and as the infrared light source, for example, a halogen lamp is used.

  As the light receiving unit 205, a spectrum analyzer is used, thereby identifying wavelengths of ultraviolet rays and infrared rays irradiated from the light emitting unit 204, and in a slurry mixed with a polishing source liquid or a plurality of polishing source liquids flowing in the pipe 201 a Detects the amount of transmitted ultraviolet and infrared light. The light emitting unit 204 emits light of a predetermined range of wavelengths of ultraviolet rays and infrared rays, and the spectrum analyzer of the light receiving unit 205 selects ultraviolet rays having a wavelength in the vicinity of 253.7 nm where the microorganisms absorb ultraviolet energy well. This transmission amount may be detected.

  In addition, the calculation means 206, the controller 207, and the notification means 208 are provided, and the output signal of the light transmission amount from the light receiving unit 205 is input to the calculation means 206, and the calculation result in the calculation means 206 is The information is input to the controller 207 to drive and control the notification unit 208 and the sterilization unit 300. The notifying means 208 is for notifying the presence or absence of microorganisms by a screen, sound or the like.

  Next, the operation of creating the slurry and supplying it to the polishing apparatuses 34 and 37 will be described with reference to FIG. In a state where the slurry mixing storage container 11 is empty, a predetermined pressure of nitrogen gas is applied from the nitrogen gas supply line 3 by opening the on-off valve 4 on the upper surface of the abrasive dispersion 2 that is the polishing stock solution in the abrasive dispersion container 1. In addition, an amount of abrasive dispersion 2 corresponding to the mixing ratio in the slurry is added to the abrasive dispersion supply line 7 through the abrasive dispersion supply pipe 6, the open on-off valve 8, and the three-way switching valve 10. To the slurry mixed storage container 11.

  After closing the on-off valve 4, the on-off valve 16 is opened on the upper surface of the hydrogen peroxide solution 14, which is a polishing stock solution in the hydrogen peroxide solution container 13, and a predetermined pressure of nitrogen gas is applied from the nitrogen gas supply line 15. Thus, an amount of the hydrogen peroxide solution 14 corresponding to the mixing ratio in the slurry is supplied from the hydrogen peroxide solution supply line 19 into the slurry mixture storage container 11 through the open on-off valve 20. Further, after closing the on-off valve 16, the on-off valve 23 is opened, and pure water which is a polishing stock solution for dilution corresponding to the mixing ratio in the slurry from the pure water supply line 21 and the pure water branch line 22 is mixed with slurry. Supply into the container 11. Each of the polishing stock solutions is supplied into the slurry mixed storage container 11, the pump 25 of the circulation line 24 is driven, and a predetermined amount is stored as the slurry 12 uniformly mixed by flow and agitation in the slurry mixed storage container 11. .

  The slurry 12 stored in a predetermined amount in the slurry mixed storage container 11 is supplied to the slurry mixed storage container 28 from the slurry supply line 26 by opening the on-off valve 27. The slurry 29 in the slurry mixing and storing container 28 circulates in the circulation line 30 by driving the pump 31, and is further supplied from the slurry supply lines 32 and 35 to the polishing apparatuses 34 and 37 by driving the pumps 33 and 36.

  The on-off valve 27 is controlled to be replenished by reducing the amount of the slurry 29 in the slurry mixing storage container 28.

  Furthermore, when the slurry 12 in the slurry mixed storage container 11 becomes empty, the above operation is repeated to store the slurry 12 in the slurry mixed storage container 11.

  During the operation of preparing the slurry and supplying it to the polishing apparatuses 34 and 37, as described above, the microorganism dispersion means 2 provided in each of the abrasive dispersion supply line 7 and the circulation lines 24 and 30 allows the abrasive dispersion 2 or Microorganisms in the slurry 12, 29 are detected.

  Here, the basic operation of the microorganism detection apparatus 200 will be described in an example in which the microorganism detection apparatus 200 is provided in the abrasive dispersion supply line 7. In the graph shown in FIG. 3, the horizontal axis represents an elapsed time, and the vertical axis represents an example of a change in transmission amount detected by the light receiving unit 205. The transmitted amounts of ultraviolet rays and infrared rays detected by the light receiving unit 205 on the vertical axis are integrated for each predetermined time from t0 to t6 in the figure. That is, the amount of transmission of ultraviolet rays and infrared rays in the respective time passages of t0 to t1, t1 to t2, t2 to t3, t3 to t4, t4 to t5, and t5 to t6 is integrated.

  The accumulated transmission amount of each of the ultraviolet rays and the infrared rays is set such that the content ratio of the abrasive grains and the irradiation amount of each light are substantially constant, and the cross-sectional area of the channel 201a, the flow velocity of the abrasive dispersion liquid, the accumulated time, etc. The predetermined conditions are optimal for discriminating abrasive grains and microorganisms.

  The abrasive dispersion liquid is supplied from the detection line 203 branched in the abrasive dispersion supply line 7 into the pipe 201a of the microorganism detection apparatus 200 and flows therethrough. Here, the abrasive dispersion liquid flowing in the pipe 201a from the light emitting unit 204 is irradiated with ultraviolet rays and infrared rays. In the state where the abrasive dispersion contains solid abrasive grains and no microorganisms are present, both the ultraviolet rays and infrared rays hitting the abrasive grains in the abrasive dispersion are not absorbed by the abrasive grains and reflected. The amount of transmission of ultraviolet rays and infrared rays that reach the dispersion liquid reaching the light receiving portion 205 is reduced compared to the amount of transmission when abrasive grains are not included. This state is indicated by A (no microorganism) in FIG. 3 and indicates the amount of transmission of the ultraviolet rays that are the first wavelength and the infrared rays that are the second wavelength between t0 to t1 and t1 to t2.

  A state in which abrasive grains are contained in the abrasive dispersion and microorganisms are present is indicated by B (with microorganisms) in FIG. 3, in each of t2 to t3, t3 to t4, t4 to t5, and t5 to t6. The integrated transmission amount of the ultraviolet rays that are the first wavelength and the infrared rays that are the second wavelength is shown.

  The infrared light having the second wavelength is transmitted through the microbial particles even if the microbial particles are present in the abrasive dispersion. As a result, the accumulated amount of infrared rays reaching the light receiving unit 205 shows the same value as in the state where no microorganism is present.

  On the other hand, the ultraviolet rays having the first wavelength are reflected and attenuated without being absorbed by the abrasive grains in the abrasive dispersion, and further absorbed by microorganisms and attenuated. As a result, the accumulated amount of ultraviolet rays reaching the light receiving unit 205 is reduced with respect to a state where no microorganism is present. Therefore, in the state indicated by B (with microorganisms) in FIG. 3, the difference between the accumulated amount of transmitted infrared rays and the accumulated amount of transmitted ultraviolet rays is larger than the state indicated by A (without microorganisms) in FIG. To do. In addition, this difference increases as the amount of microorganisms present in the abrasive dispersion increases. The difference in the transmission amount is calculated by the calculation means 206.

  As described above, the microorganism detection device of the present invention includes the light emitting unit 204 that irradiates the abrasive dispersion, which is the liquid to be measured flowing in the tube body 201, with the ultraviolet light that is the first wavelength, and the first wavelength. A light receiving unit 205 that detects the amount of ultraviolet light transmitted by microorganisms and the amount of transmitted light by abrasive grains that are solids other than microorganisms, and further, infrared light that is the second wavelength in the abrasive dispersion that is the liquid to be measured. A light emitting unit 204 for irradiating light, a light receiving unit 205 for detecting the amount of transmission of abrasive grains other than microorganisms of infrared light having the second wavelength, and microorganisms by irradiation of ultraviolet light having the first wavelength And calculating means 206 for calculating the difference between the transmission amount of abrasive grains that are solids other than microorganisms and the transmission amount of abrasive grains that are solids other than microorganisms by irradiation with infrared light having the second wavelength. Depending on the transmission amount difference calculated by the calculation means. It is intended to detect the presence of microorganisms.

  That is, the abrasive dispersion, which is a fluid to be measured, is irradiated with light having different wavelengths of ultraviolet light as the first wavelength and infrared light as the second wavelength, and the amount of light transmitted through the ultraviolet light as the first wavelength; The presence of microorganisms can be continuously detected in an on-line state of the slurry supply apparatus based on a difference from the amount of transmitted light in the infrared light having the second wavelength.

  Further, the transmission amount of each wavelength is an integrated value in a predetermined amount of the liquid to be measured that flows, so that it is possible to accurately detect even a very small amount of microorganisms.

  Further, by measuring the transmission amount of the first wavelength light and the second wavelength light with a spectrum analyzer, the transmission amount of each light can be continuously measured with high accuracy.

  Furthermore, by using light of the first wavelength as ultraviolet light and light of the second wavelength as infrared light, it is possible to reliably identify microorganisms and solids other than microorganisms.

  In addition, by providing an informing means for informing the presence of microorganisms, it is possible to always grasp the presence of microorganisms in the liquid to be measured and to perform a prompt treatment corresponding to this.

  In addition, when the microorganisms are detected by the microorganism detection device by detecting microorganisms in any part from the supply line of the polishing stock solution to the supply line of the slurry that is a mixed liquid of the plurality of polishing stock solutions to the polishing device Therefore, it is possible to respond quickly so as not to adversely affect the polishing apparatus. Therefore, it is possible to always maintain stable polishing in the polishing apparatus.

  In addition, a plurality of parts from the polishing stock solution supply line to the supply line to the polishing apparatus for slurry, which is a mixed solution of the plurality of polishing stock solutions, are provided with a microorganism detecting device, so that In the supply line to the polishing apparatus of the slurry, which is a mixed solution of the polishing stock solution, a site where microorganisms are present or a breeding site can be specified.

  The microorganism detection apparatus 200 located on a supply line 203 that is branched from each of the circulation lines 24 and 30 includes a slurry (mixed polishing liquid) 12 in the slurry mixed storage container 11 or a slurry in the slurry mixed storage container 28 ( Mixed polishing liquid) 29 flows through the supply line 203. Similarly to the basic operation of the microorganism detection apparatus 200 in the example provided in the abrasive dispersion supply line 7, microorganisms in the slurry that is a mixed liquid of a plurality of polishing source liquids can also be detected.

  In addition, the site | part which provided the microorganisms detection apparatus 200 is not limited to the said structure, For example, you may provide in each of the slurry supply lines 26, 32, and 35. FIG.

  Further, although the light receiving unit 205 is a spectrum analyzer, the present invention is not limited to this, and elements that individually receive ultraviolet rays and infrared rays may be used. Furthermore, the light having the second wavelength is not limited to infrared light as long as it has a property of transmitting without being absorbed by the microorganisms and being reflected by the abrasive grains and reflected and attenuated.

  In addition, the light emitting unit 204 positions an ultraviolet light source and an infrared light source at a predetermined distance in the flow direction of the slurry that is a polishing source liquid or a mixture of polishing source liquids, and positions the light receiving unit 205 to face the light emitting unit 204. You may let them. In this case, the amount of transmitted light in the slurry, which is the same polishing stock solution flowing in the tube 201 or a mixed solution of the polishing stock solution, is measured. This is done by setting the detection start timing of ultraviolet and infrared rays according to the distance between the ultraviolet and infrared light sources and the flow rate of the polishing stock solution or slurry.

  In the embodiment, the difference between the amount of transmitted light of the first wavelength ultraviolet ray and the second wavelength infrared ray is calculated as an integrated difference. The transmission amount of each wavelength light in the slurry which is the same polishing source liquid or a mixture of the polishing source liquids may be continuously measured in real time to calculate the difference in transmission amount.

  Next, the operation of the sterilizing means 300 will be described. When microorganisms are not detected by the microorganism detection apparatus 200, this is notified by the notification means 208. Further, in order to avoid wasting power due to unnecessary ultraviolet irradiation, the sterilization means 300 is not given an ultraviolet irradiation instruction from the controller 207, and the normal operation of the slurry supply apparatus is continued. When the presence of microorganisms is detected, this is notified by the notification means 208 and the sterilization means 300 is driven by an instruction from the control means 207. Furthermore, the sterilizing means 300 provided on the downstream side of the microorganism detection apparatus 200 irradiates the abrasive dispersion 2 passing therethrough with ultraviolet rays to kill the microorganisms. Thereby, the flow of microorganisms to the downstream area of the sterilization means 300 can be prevented.

  Further, the sterilizing means 300 has a function of suppressing the increase of microorganisms as well as bacteria or killing microorganisms. Ultraviolet rays are applied to the slurry which is the particle dispersion 2 or the mixed polishing liquid, and the strength thereof is increased. Irradiate while adjusting. The sterilizing means 300 is not limited to ultraviolet irradiation, and may be other means such as heating to a predetermined temperature.

  By changing the irradiation amount of ultraviolet rays necessary for killing the microorganisms in the sterilization means 300 according to the detection level of microorganisms within a predetermined range of the microorganism detection apparatus 200, the microorganisms are killed even if the number of microorganisms varies. Can do. Moreover, the killing effect of the microorganisms by the sterilization means 300 provided in the abrasive dispersion supply line 7 can be confirmed by the detection of microorganisms by the microorganism detection device 200 provided in each of the circulation lines 24 and 30.

  Further, when the microorganisms in the slurry 12 and 29 are detected by the microorganism detection device 200 provided in each of the circulation lines 24 and 30, this is notified by the notification means 208. Further, the sterilization means 300 provided on the downstream side of the microorganism detection means 200 irradiates the slurry 12 and 29 passing therethrough with ultraviolet rays to kill the microorganisms. Further, the effect of killing microorganisms by the sterilization means 300 provided in the circulation line 24 can be confirmed by detection of microorganisms by the microorganism detection device 200 provided in the circulation line 30.

  Although the sterilization means 300 is provided on the downstream side of the microorganism detection apparatus 200, a plurality of microorganism detection apparatuses 200 may be provided on the downstream side and the upstream side in the vicinity of the sterilization means 300. In this case, microorganisms can be detected by the upstream microorganism detection apparatus 200, and the sterilization effect of the sterilization means 300 can be confirmed by the downstream microorganism detection apparatus 200 after passing through the sterilization means 300.

  In the first embodiment, a plurality of microorganism detecting devices 200 are provided in a region from the supply line of the polishing stock solution to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing device. It may be. For example, the microorganism detecting apparatus 200 may be provided here if the most easily contaminated or breeding part can be identified. Further, the microorganism detecting device 200 may be provided in the circulation line 30 located upstream immediately before the polishing devices 34 and 37.

  As described above, in the embodiment of the present invention, a microorganism that detects microorganisms in any part from the supply line of the polishing stock solution to the supply line of the slurry that is a mixed liquid of the plurality of polishing stock solutions to the polishing apparatus. A detection device 200 is provided.

  Accordingly, microorganisms in the slurry supply line that is a mixed liquid of the plurality of polishing stock solutions can be always continuously detected from the polishing stock solution supply line, and when the microorganisms are detected by the microorganism detection apparatus 200, This makes it possible to quickly respond such as stopping the polishing apparatus, driving a sterilizing means for killing microorganisms, and cleaning for removing microorganisms. Therefore, it is possible to provide a slurry supply apparatus that can perform stable polishing.

  Further, the plurality of parts from the polishing stock solution supply line to the supply line to the polishing apparatus for the slurry, which is a mixed solution of the plurality of polishing stock solutions, are provided with the microorganism detection device 200, so In the supply line to the polishing apparatus of the slurry, which is a mixed solution of the polishing stock solution, a site where microorganisms are present or a breeding site can be specified.

  Further, by providing the notification means 208, the presence and level of microorganisms in the supply line from the polishing stock solution supply line to the slurry polishing apparatus, which is a mixed solution of the plurality of polishing stock solutions, are always reliably grasped at all times. In addition, it is possible to implement a prompt treatment corresponding to this.

Further, at least a part of the polishing stock solution from the supply line of the polishing stock solution to the supply line to the polishing apparatus of the slurry which is a mixed solution of the plurality of polishing stock solutions is provided with sterilizing means for sterilizing microorganisms,
The sterilization means is driven based on detection of microorganisms by the microorganism detection apparatus.

  This stabilizes the polishing of the wafer by preventing the discharge of microorganisms to the polishing apparatus, and prevents the change in flow rate due to the increase in flow resistance in the polishing fluid supply path due to the growth of microorganisms, thus stabilizing the mixing ratio. Can be achieved. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.

  In the process of continuously operating the slurry supply apparatus, the microorganism detection apparatus 200 may detect the continued detection and increase tendency of microorganisms. This is because there is a possibility that microorganisms are attached and propagated in any part from the supply line of the polishing stock solution to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing apparatus.

When microorganisms adhere and propagate, there is a possibility that the fluctuation of the mixing ratio of a plurality of polishing stock solutions or the amount of slurry supplied to the polishing apparatus will change, which will adversely affect the polishing performance of the polishing apparatus.
For this reason, it is necessary to remove attached and propagated microorganisms.

  For this reason, when the microorganism detection apparatus 200 detects a continuous detection or increase tendency of microorganisms, cleaning is performed to remove attached and propagated microorganisms. This cleaning means and each step at the time of cleaning will be described in order with reference to FIGS. 4 to 9 by taking as an example the case of removing microorganisms in the abrasive dispersion supply line 7.

  The removal of microorganisms and the cleaning operation are performed within a time until the slurry 12 in the slurry mixed storage container 11 becomes empty after the slurry 12 is created in the slurry mixed storage container 11. Supply of the slurry 12 and 29 to 34 and 37 is in a continuous state.

  FIG. 4 shows the state of the first step during cleaning, which is a state of discharging the abrasive dispersion 2 in the abrasive dispersion supply line 7 by supplying pure water. In FIG. Are given the same numbers and their explanation is omitted. The difference from FIG. 1 is that the abrasive dispersion container 1 is moved apart at the part of the detachable member 5 and the receiving container 58 for receiving the abrasive dispersion 2 discharged from the abrasive dispersion supply pipe 6 is positioned. It is a configuration. In addition, the solid line arrow in a figure shows the flow of pure water.

  Pure water is supplied from the pure water supply line 21 into the abrasive dispersion supply line 7 through the branch line 56, the open on-off valve 57, and the three-way switching valves 43 and 10. Pure water flows through the on-off valve 8 with the abrasive dispersion supply line 7 open and the abrasive dispersion supply pipe 6, thereby receiving the abrasive dispersion 2 in the abrasive dispersion supply line 7 and discharging it to the container 58. At the same time, the inside of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 is once cleaned with pure water. When the inside of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 is replaced with pure water, and when a predetermined amount of pure water has flowed into the receiving container 58, the open / close valve 57 is closed to supply pure water. Stop. At this time, the open / close valve 42 of the related flow path is closed, and each of the three-way switching valves 43 and 10 controls the flow path in the direction indicated by the solid line arrow in the figure.

  FIG. 5 shows the state of the second step at the time of supplying the TMAH liquid 39 into the abrasive dispersion supply line 7. In FIG. 3, the same parts as those in FIGS. Is omitted. 1 and 4, the receiving container 59 for receiving the TMAH liquid discharged from the abrasive dispersion supply pipe 6 is positioned. In addition, the solid line arrow in a figure shows the flow of TMAH liquid, and the broken line arrow shows the flow of nitrogen gas.

  As described above, a predetermined amount of the TMAH liquid 39 is stored in the TMAH liquid container 38, and the TMAH liquid supply line 40 opened in the TMAH liquid container 38 includes the three-way switching valve 41, the on-off valve 42, the three-way switching valve 43, the cleaning liquid. It is connected to the three-way switching valve 10 via a supply line 44. At this time, the on-off valve 8 is opened, the on-off valves 48, 57 related to the flow path of the TMAH liquid 39 are closed, and each of the three-way switching valves 41, 43, 10 flows in the direction indicated by the solid line arrow in the figure. The road is controlled.

  The on-off valve 46 is opened from the nitrogen gas supply line 45 and the supply pressure of nitrogen gas is applied to the upper surface of the TMAH liquid 39 in the TMAH liquid container 38. The TMAH liquid 39 in the TMAH liquid container 38 is pushed out to the TMAH liquid supply line 40, and passes through the three-way switching valve 41, the open on-off valve 42, the three-way switching valve 43, the cleaning liquid supply line 44, and the three-way switching valve 10. It flows into the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6. As a result, the pure water in the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 is pushed out and replaced with the TMAH liquid 39. Pure water and TMAH liquid 39 flow out from the abrasive dispersion supply pipe 6 to the receiving container 59.

  When the abrasive dispersion liquid supply line 7 and the abrasive dispersion liquid supply pipe 6 are replaced with the TMAH liquid 39, the on-off valves 46 and 42 are closed to stop the supply of the TMAH liquid 39 and the abrasive dispersion liquid. The TMAH liquid is retained and held in the supply line 7 and the abrasive dispersion supply pipe 6 for a predetermined time (for example, 5 to 10 minutes). At this time, in the process in which the TMAH liquid which is an organic strong alkaline substance is in contact with the microorganisms which have adhered and propagated to the inner walls of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6, the cells of the microorganisms are dissolved. Sterilize. As a result, the TMAH solution 85, which is an organic strong alkali substance, sufficiently contacts and penetrates the microorganisms that adhere to and propagate on the inner wall of the supply line having the bent portion and are partially agglomerated. Cells can be lysed and sterilized. In addition, the microorganisms are negatively charged due to the change in pH to the alkali side due to the supply of the TMAH solution, and the microorganisms are electrically repelled by the inner wall of the particle dispersion supply line 7 and the abrasive dispersion supply tube 6 made of a resin material. Physical delamination also occurs. The TMAH solution 39 is not particularly limited, but is used after being diluted with ultrapure water to a concentration of 25%. It is used as the mainstream of developer in semiconductor factories and can be shared as a whole semiconductor manufacturing facility.

  As described above, by discharging the abrasive dispersion 2 from the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 and cleaning with pure water, the abrasive dispersion supply line 7, the abrasive The components of the abrasive dispersion 2 are removed from the surface of the microorganisms that have adhered and propagated on the inner wall and the inner wall of the particle dispersion supply pipe 6, and the TMAH solution 39 directly contacts and penetrates the microorganisms. Can be dissolved and sterilized.

  The pure water in the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 was supplied by pushing out the TMAH liquid 39 and replaced with the TMAH liquid 39. After the pure water in the dispersion liquid supply line 7 and the abrasive dispersion liquid supply pipe 6 is discharged, the TMAH liquid may be supplied.

  FIG. 6 shows a state of the third step at the time of cleaning to discharge the TMAH liquid 39 in the abrasive dispersion supply line 7 by nitrogen gas supply. In FIG. 4, the same parts as those in FIGS. The description is omitted. In addition, the broken line arrow in a figure shows the flow of nitrogen gas. After the TMAH liquid is retained and held in the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 for a predetermined time, the on-off valve 46 and the on-off valve 57 are closed, the on-off valve 42, the on-off valve 48, and the on-off valve 8 is opened. The three-way switching valves 41, 43, and 10 control the flow paths in the nitrogen gas flow direction shown in FIG. The nitrogen gas is supplied from the nitrogen gas supply line 45 to the branch line 47, the opening / closing valve 48, the three-way switching valve 41, the opening / closing valve 42, the three-way switching valve 43, the three-way switching valve 10, and the cleaning liquid supply line 44. 7 and supplied into the abrasive dispersion supply pipe 6. As a result, the TMAH liquid 39 staying in the cleaning liquid supply line 44, the abrasive dispersion supply line 7, and the abrasive dispersion supply pipe 6 is discharged to the receiving container 59 through the opening / closing valve 8.

  FIG. 7 shows the state of the fourth step during cleaning for supplying hydrogen peroxide solution into the abrasive dispersion supply line 7. In FIG. 5, the same parts as those in FIGS. Description is omitted. A difference from FIGS. 1 and 6 is that a receiving container 60 for receiving the hydrogen peroxide solution discharged from the abrasive dispersion supply pipe 6 is located. In the figure, solid arrows indicate the flow of hydrogen peroxide water, and broken arrows indicate the flow of nitrogen gas.

As described above, a predetermined amount of hydrogen peroxide solution (H ₂ O ₂ ) 50 is stored in the hydrogen peroxide solution container 49, and the hydrogen peroxide solution supply line 51 opened in the hydrogen peroxide solution container 49 has three sides. The three-way switching valve 10 is connected via a switching valve 41, an on-off valve 42, a three-way switching valve 43, and a cleaning liquid supply line 44. At this time, the on-off valve 8 is opened, the on-off valves 55 and 57 related to the flow path of the hydrogen peroxide solution 50 are closed, and each of the three-way switching valves 41, 43, and 10 is in the direction indicated by the solid arrow in the figure. The flow path is controlled.

  The on-off valve 53 is opened from the nitrogen gas supply line 52, and the supply pressure of nitrogen gas is applied to the upper surface of the hydrogen peroxide solution 50 in the hydrogen peroxide solution container 49. The hydrogen peroxide solution 50 in the hydrogen peroxide solution container 49 is pushed out to the hydrogen peroxide solution supply line 51, and the three-way switching valve 41, the open on-off valve 42, the three-way switching valve 43, the cleaning liquid supply line 44, and the three-way switching. It flows to the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 through the valve 10. Further, it flows out from the abrasive dispersion supply pipe 6 to the receiving container 60 through the on-off valve 8.

  At the stage where the abrasive dispersion liquid supply line 7 and the abrasive dispersion supply pipe 6 are filled with the hydrogen peroxide solution 50, the on-off valves 53 and 42 are closed to stop the supply of the hydrogen peroxide solution 50, The hydrogen peroxide solution 50 is retained and held in the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 for a predetermined time (for example, 5 to 10 minutes).

  At this time, the TMAH liquid 39, which is a strong alkaline substance that remains attached to microorganisms, reacts with the hydrogen peroxide solution 50 and fires due to the reaction between the abrasive dispersion supply line 7, the inner wall of the abrasive dispersion supply pipe 6, and the microorganisms. Separation of microorganisms dissolved by the TMAH liquid from the inner walls of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 and sterilization of the inner walls of the supply line can be further promoted.

  The hydrogen peroxide solution 50 is used in a semiconductor factory and can be shared as a whole semiconductor manufacturing facility.

  FIG. 8 shows the state of the fifth step during cleaning, which is a state in which the hydrogen peroxide solution 50 in the abrasive dispersion supply line 7 by pure water supply is discharged. In FIG. The same parts are denoted by the same reference numerals and the description thereof is omitted. In addition, the solid line arrow in a figure shows the flow of pure water.

  Pure water is supplied from the pure water supply line 21 into the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 through the branch line 56, the open on-off valve 57, and the three-way switching valves 43 and 10. The pure water flows through the on-off valve 8 and the abrasive dispersion supply pipe 6 that are opened in the abrasive dispersion supply line 7, and thereby the hydrogen peroxide solution 50 in the abrasive dispersion supply line 7 is received in the container 60. While discharging, the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 are cleaned with pure water. When a predetermined amount of pure water flows out from the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 into the receiving container 60, the on-off valve 57 is closed to stop the supply of pure water. At this time, the open / close valve 42 of the related flow path is closed, and each of the three-way switching valves 43 and 10 controls the flow path in the direction indicated by the solid line arrow in the figure. As a result, microorganisms adhering to the inner walls of the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 are discharged together with the hydrogen peroxide solution 50 and pure water into the receiving container 60.

  FIG. 9 shows the state of the sixth step during cleaning for discharging pure water in the abrasive dispersion supply line 7 by nitrogen gas supply. In FIG. 7, the same parts as those in FIGS. The description is omitted. In addition, the broken line arrow in a figure shows the flow of nitrogen gas.

  After the hydrogen peroxide solution 50 in the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 is discharged and washed with pure water, the on-off valve 46 and the on-off valve 57 are closed, the on-off valve 42 and the on-off valve 48. The on-off valve 8 is opened. The three-way switching valves 41, 43 and 10 control the flow paths in the nitrogen gas flow direction shown in FIG. The nitrogen gas is supplied from the nitrogen gas supply line 45 to the branch line 47, the opening / closing valve 48, the three-way switching valve 41, the opening / closing valve 42, the three-way switching valve 43, the three-way switching valve 10, and the cleaning liquid supply line 44. 7 and supplied into the abrasive dispersion supply pipe 6. As a result, pure water in the cleaning liquid supply line 44, the abrasive dispersion supply line 7, and the abrasive dispersion supply pipe 6 is discharged to the receiving container 60 through the on-off valve 8.

  The microorganism removal and cleaning operations are completed by the first to sixth steps. The abrasive dispersion container 1 for storing the abrasive dispersion 2 again is attached to the detachable member 5, and the slurry is produced as shown in FIG.

  In the embodiment, each on-off valve, three-way switching valve, and pump constituting the slurry supply device are individually controlled by a controller (not shown). Further, the abrasive dispersion liquid 2, the hydrogen peroxide solutions 14, 50, and the TMAH liquid 39 are supplied by means of pressurization with nitrogen gas, but supply means by a pump, a drop pressure, or the like may be used. Furthermore, the number of polishing stock solutions for slurry, the components, and the configuration of the slurry supply device are merely examples, and the present invention is not limited thereto. Further, in the cleaning step, the TMAH solution 39, the hydrogen peroxide solution 50, pure water, and nitrogen gas are supplied from the opposite direction (reverse direction) of the abrasive dispersion 2 to the abrasive dispersion supply pipe 6 and the abrasive dispersion supply line. Although it was made to supply and flow to 7, it may be the same direction. The abrasive dispersion container 1 is exchanged with the new abrasive dispersion container 1 containing the abrasive dispersion 2 via the detachable member 5 when the abrasive dispersion 2 becomes empty. Therefore, the containers 58, 59, and 60 that receive the abrasive dispersion 2, the TMAH 39, the hydrogen peroxide solution 50, and the pure water are also exchanged via the detachable member 5 in the same manner as the abrasive dispersion container 1 at the time of cleaning. Therefore, the TMAH solution 39, the hydrogen peroxide solution 50, pure water, and nitrogen gas can be supplied from the opposite direction (reverse direction) to the abrasive dispersion 62 flow. It is preferable to feed and flow to the tube 6 and the abrasive dispersion supply line 7.

  Further, in the embodiment, the example of removing and cleaning microorganisms adhering in the abrasive dispersion supply line 7 has been described, but polishing of a slurry which is a mixed liquid of the plurality of polishing stock solutions from the polishing stock solution supply line. Slurry supply lines 26, 32, 32, 35, and circulation lines 24, 30, each of the slurry mixed storage container 11 and the slurry mixed storage container 28, which are at least a part of the supply line to the apparatus The basic microorganism removal and cleaning operations of the first to sixth steps can be similarly performed.

  As described above, the TMAH liquid 39 is supplied to and discharged from at least a part of the polishing stock solution from the supply line to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing apparatus. The present invention is a slurry supply apparatus cleaning method characterized in that hydrogen water 50 is supplied and discharged, and a slurry supply apparatus using this cleaning method.

  As a result, microorganisms adhered and propagated by the TMAH solution are dissolved, and further, the removal of the microorganisms by the reaction between the TMAH solution and the hydrogen peroxide solution is promoted, so that the microorganisms can be reliably removed and washed. Therefore, it is possible to prevent a change in flow rate due to an increase in flow resistance in the polishing fluid supply path due to the propagation of microorganisms, and to stabilize the mixing ratio. Further, it is possible to improve and stabilize the accuracy of the amount of slurry supplied to the polishing apparatus.

  In addition, by supplying the TMAH liquid and retaining it in the supply line for a predetermined time, TMAH, which is an organic strong alkaline substance, is added to the microorganisms that adhere to and propagate on the inner wall even in the bent part of the supply line and partly become agglomerated. The liquid can be sufficiently contacted and penetrated to lyse and sterilize microbial cells more reliably.

  Also, by supplying hydrogen peroxide water and retaining it in the supply line for a predetermined time, the tetramethylammonium hydroxide liquid, which is a strong alkaline substance that remains attached to the inner wall of the supply line and the microorganisms, reacts with the hydrogen peroxide water. It is possible to further promote peeling of the microorganisms that have been fired and dissolved by the TMAH solution from the inner wall and sterilization of the inner wall of the supply line.

As described above, the microorganisms adhere to and propagate on the abrasive dispersion supply pipe 6 and the abrasive dispersion supply line 7 as time passes when the slurry 12 is created in the slurry mixing storage container 11. For this reason, removal and washing of microorganisms adhering to and growing on the abrasive dispersion supply line 7 may be performed at predetermined intervals within a permissible range in which the mixing ratio of the plurality of polishing stock solutions does not adversely affect the polishing performance of the polishing apparatus. Good.

  In addition, microorganism removal and cleaning operations are performed by detecting the pressure on the upstream and downstream sides of the abrasive dispersion supply pipe 6 and the abrasive dispersion supply line 7 (not shown), thereby causing the flow of microorganisms due to adhesion and propagation. When the road resistance has increased by a predetermined value or more, it is possible to determine when to perform the microorganism removal and cleaning operations. In this case, it is possible to more surely grasp the time required for removing and washing the microorganisms.

  Next, another configuration of the first embodiment will be described with reference to FIG. This is a microbe detection apparatus that removes the polishing stock solution or slurry from a plurality of sites from a supply line of the polishing stock solution to a supply line of slurry that is a mixed liquid of the plurality of polishing stock solutions. 200 is used to detect microorganisms. The same reference numerals as those in FIG.

  The switching line 400 is connected to the detection line 7 a branched from the abrasive dispersion supply line 7, and the switching valve 400 and the microorganism detection device 200 are further connected. The sterilizing means 300 is provided on the downstream side of the abrasive dispersion supply line 7 where the detection line 209 branches.

  Further, the detection line 24a branched from the circulation line 24 is connected to the switching valve 400, and the switching valve 400 and the microorganism detection device 200 are further connected. The sterilizing means 300 is provided on the downstream side of the circulation line 24 where the detection line 209 branches.

  Furthermore, the switching line 400 is connected to the detection line 30a branched from the circulation line 30, and the switching valve 400 and the microorganism detection device 200 are further connected. The sterilizing means 300 is provided on the downstream side of the circulation line 30 where the detection line 209 branches.

  In the above-described configuration, the flow path is switched by the switching valve 400 to sequentially detect the abrasive dispersion 2 from the abrasive dispersion supply line 7, the slurry 12 from the circulation line 24, and the slurry 29 from the circulation line 30. 200. The operations of the microorganism detection apparatus 200 and the sterilization means 300 are the same as those described above, and a description thereof is omitted.

  Thereby, in the supply line from the supply line of the polishing stock solution to the polishing apparatus for the slurry, which is a mixed solution of the plurality of polishing stock solutions, the number of microorganism detecting means is reduced and the site where the microorganisms are present or the breeding site is specified. Can do.

(Example 2)
Hereinafter, the slurry supply apparatus of Example 2 of this invention is demonstrated, referring FIGS. 11-18.

  A fundamental difference from the first embodiment is that a plurality of polishing stock solutions are mixed as much as possible immediately before the polishing apparatus and supplied to the polishing apparatus without providing a container for storing a predetermined amount of slurry. FIG. 11 is a basic configuration diagram of the slurry supply apparatus of the present invention, FIG. 12 is a configuration diagram of the slurry supply apparatus showing the state of the first step during cleaning for discharging the abrasive dispersion by supplying pure water, and FIG. 13 is a TMAH solution FIG. 14 is a configuration diagram of the slurry supply apparatus showing the state of the third step during cleaning to discharge the TMAH liquid by nitrogen gas supply, FIG. 15 is a configuration diagram of the slurry supply apparatus showing the state of the fourth step at the time of cleaning to supply the hydrogen peroxide solution, and FIG. 16 shows the state of the fifth step at the time of cleaning to discharge the hydrogen peroxide solution by supplying pure water. FIG. 17 is a configuration diagram of the slurry supply device, FIG. 17 is a configuration diagram of the slurry supply device showing the state of the sixth step during the cleaning to discharge pure water by supplying nitrogen gas, and FIG. is there.

  In FIG. 11, the basic configuration will be described first. A predetermined amount of the abrasive dispersion 62 is stored in the abrasive dispersion container 61, and nitrogen gas is supplied from the nitrogen gas supply line 63 through the opening / closing valve 64 to the upper surface of the abrasive dispersion 62 in the abrasive dispersion container 61. Pressurize. A supply pipe 66 is provided in the abrasive dispersion container 61 and communicates with the abrasive dispersion supply line 67. The nitrogen gas supply line 63 and the abrasive dispersion liquid supply line 67 are fixed to the detachable member 65 and configured to be detachable from the abrasive dispersion container 61.

  The abrasive dispersion 62 is supplied to the mixer 70 via the on-off valve 69 and the flow meter 68 of the abrasive dispersion supply line 67. The abrasive dispersion supply line 67 is installed with a plurality of bent portions in the mounted state. An abrasive dispersion 62, a hydrogen peroxide solution to be described later, and pure water as needed are supplied into the mixer 70, and mixing thereof is promoted to create a slurry that is a mixed polishing liquid.

  The hydrogen peroxide solution 72 is stored in the hydrogen peroxide solution container 71, and the upper surface of the hydrogen peroxide solution 72 in the hydrogen peroxide solution container 71 is pressurized with nitrogen gas from the nitrogen gas supply line 73 through the on-off valve 74. . A supply pipe 76 is provided in the hydrogen peroxide solution container 71 and communicates with the hydrogen peroxide solution supply line 77. Further, the nitrogen gas supply line 73 and the hydrogen peroxide solution supply line 77 are fixed to the detachable member 75 and are configured to be detachable from the hydrogen peroxide solution container 71. A hydrogen peroxide solution 72 is supplied to the mixer 70 via the on-off valve 79 of the hydrogen peroxide solution supply line 77.

  The mixed slurry is supplied from the mixer 70 via the slurry supply line 80 and the three-way switching valve 81 to the polishing unit 88 via the slurry discharge line 82.

  A TMAH liquid 85 is stored in a predetermined amount in the TMAH liquid container 84, and a TMAH liquid supply line 90 opened in the TMAH liquid container 84 is passed through a three-way switching valve 91, a three-way switching valve 92, and a cleaning liquid supply line 93. It is connected to the. Nitrogen gas is pressurized from the nitrogen gas supply line 86 through the on-off valve 87 to pressurize the upper surface of the TMAH liquid 85 in the TMAH liquid container 84. A branch line 88 branched from the nitrogen gas supply line 86 is connected to a TMAH liquid supply line 90 via an on-off valve 89.

  A predetermined amount of hydrogen peroxide solution 95 is stored in the hydrogen peroxide solution container 94, and a hydrogen peroxide solution supply line 96 opened in the hydrogen peroxide solution container 94 is connected to the three-way switching valve 91. Nitrogen gas is pressurized from the nitrogen gas supply line 97 through the on-off valve 98 to pressurize the upper surface of the hydrogen peroxide solution 95 in the hydrogen peroxide solution container 94. A branch line 99 branched from the nitrogen gas supply line 97 is connected to the hydrogen peroxide solution supply line 96 via the on-off valve 100 and is connected to the cleaning liquid supply line 93 via the three-way switching valve 91 and the three-way switching valve 92. A branch line 99 branched from the pure water supply line is connected to the three-way switching valve 10 via the on-off valve 102.

  A microorganism detection device 200 is provided in the slurry supply line 80 extending from the three-way switching valve 81 and the polishing device 83 of the slurry supply line 80, and a sterilizing means 300 is provided downstream of the microorganism detection device 200. The microorganism detecting device 200 and the sterilizing means 300 are the same as those used in the first embodiment, and a description thereof is omitted.

  Next, the preparation of the slurry and the supply operation to the polishing unit 83 will be described. A predetermined pressure of nitrogen gas is applied from the nitrogen gas supply line 63 by opening the opening / closing valve 64 on the upper surface of the abrasive dispersion liquid 62 in the grain dispersion container 61, whereby an amount of abrasive dispersion corresponding to the mixing ratio in the slurry is applied. The liquid 62 is supplied into the mixer 70 from the abrasive dispersion supply line 67 as an open / close valve 69.

  At the same time as the supply of the abrasive dispersion 62 is started, the open / close valve 74 is opened on the upper surface of the hydrogen peroxide solution 72 in the hydrogen peroxide solution container 71 to apply a predetermined pressure of nitrogen gas from the nitrogen gas supply line 73. Thus, an amount of hydrogen peroxide solution 72 corresponding to the mixing ratio in the slurry is supplied from the hydrogen peroxide solution supply line 77 into the mixer 70 through the open on-off valve 20. The abrasive dispersion 62 and the hydrogen peroxide solution 72 are uniformly mixed in a mixer 70, and a slurry as a mixed polishing liquid is passed through a three-way switching valve 81 from a slurry supply line 80 and a slurry discharge line 82 to a polishing unit 83. To supply. The mixing ratio of the abrasive dispersion 62 and the hydrogen peroxide solution is measured and managed by the respective flow meters 68 and 76, and is controlled to a predetermined component ratio.

  During the preparation of the slurry and the supply operation to the polishing device 83, as described above, the slurry is supplied from the detection line 203 branched from the slurry supply line 80 to the microorganism detection device 200, thereby detecting the microorganisms in the slurry.

  Next, the sterilization means 300 and this operation will be described. When microorganisms are not detected by the microorganism detection apparatus 200, this is notified by the notification means 208a. Further, in order to avoid wasting power due to unnecessary ultraviolet irradiation, the sterilization means 300 is not given an ultraviolet irradiation instruction from the controller 207, and the normal operation of the slurry supply apparatus is continued. Further, when the presence of the microorganism is detected, this is notified by the notification means 208a, and the sterilization means 300 is operated by an instruction from the control means 207. Furthermore, the sterilizing means 300 provided on the downstream side of the microorganism detection apparatus 200 irradiates the abrasive dispersion 2 passing therethrough with ultraviolet rays to kill the microorganisms. Thereby, the flow of microorganisms to the downstream area of the sterilization means 300 can be prevented.

  Although the sterilization means 300 is provided on the downstream side of the microorganism detection apparatus 200, a plurality of microorganism detection apparatuses 200 may be provided on the downstream side and the upstream side in the vicinity of the sterilization means 300. In this case, microorganisms can be detected by the upstream microorganism detection apparatus 200, and the sterilization effect of the sterilization means 300 can be confirmed by the downstream microorganism detection apparatus 200 after passing through the sterilization means 300.

  In Example 2, one microorganism detecting device 200 is provided in a portion that reaches the supply line to the polishing device for slurry, which is a mixed solution of the plurality of polishing stock solutions. However, the slurry supply line 80 and the abrasive grains are provided. The dispersion liquid supply line 67 may be provided at a plurality of locations.

  As described in the first embodiment, when the microorganism detection apparatus 200 detects a continuous detection or increase tendency of microorganisms, cleaning is performed to remove attached and propagated microorganisms. This cleaning means and each step at the time of cleaning will be described in order with reference to FIGS.

  FIG. 12 shows the state of the first step during cleaning, which is a state in which the abrasive dispersion 2 in the abrasive dispersion supply line 7 by pure water supply is discharged. In FIG. Are given the same numbers and their explanation is omitted. The difference from FIG. 11 is that the abrasive dispersion liquid container 61 is moved apart at the detachable member 65 and the receiving container 103 that receives the abrasive dispersion 62 discharged from the supply pipe 66 is positioned. It is. In addition, the solid line arrow in a figure shows the flow of pure water.

  Pure water is supplied from the pure water supply line 101 into the slurry supply line 80 and the abrasive dispersion supply line 67 through the open on-off valve 102 and the three-way switching valves 92 and 81. Pure water flows to the slurry supply line 80, the mixer 70, the abrasive dispersion supply line 67, the open on-off valve 69, the flow meter 68, and the abrasive dispersion supply pipe 6, whereby the abrasive dispersion 2 is discharged. It is discharged into the receiving container 103 and washed once with pure water. Further, when pure water is allowed to flow into the receiving container 103, the on-off valve 102 is closed to stop the supply of pure water. At this time, each of the three-way switching valves 92 and 81 of the related flow path controls the flow path in the direction indicated by the solid line arrow in the figure.

  FIG. 13 shows the state of the second step at the time of supplying the TMAH solution 85 into the slurry supply line 80 and the abrasive dispersion supply line 67. In FIG. 13, the same parts as those in FIGS. A number is attached and explanation is omitted. 11 and 12, the receiving container 104 for receiving the TMAH liquid discharged from the supply pipe 66 is positioned. In addition, the solid line arrow in a figure shows the flow of TMAH liquid, and the broken line arrow shows the flow of nitrogen gas.

  As described above, a predetermined amount of TMAH liquid 85 is stored in the TMAH liquid container 84, and the TMAH liquid supply line 90 opened in the TMAH liquid container 84 is switched three-way through the three-way switching valves 91 and 92 and the cleaning liquid supply line 93. Connected to the valve 81. At this time, the on-off valve 69 is opened, the on-off valve 89 related to the flow path of the TMAH liquid 85 is closed, and each of the three-way switching valves 91, 92, 81 has a flow path in the direction indicated by the solid line arrow in the figure. It is what is being controlled.

  The on-off valve 87 is opened from the nitrogen gas supply line 86 and the supply pressure of nitrogen gas is applied to the upper surface of the TMAH liquid 85 in the TMAH liquid container 84. The TMAH liquid 85 in the TMAH liquid container 84 is pushed out to the TMAH liquid supply line 90 and is supplied to the slurry supply line 80 and the abrasive dispersion liquid via the three-way switching valves 91 and 92, the cleaning liquid supply line 93, and the three-way switching valve 81. It flows to the line 67 and the supply pipe 66. As a result, the pure water in the slurry supply line 80, the abrasive dispersion supply line 67, and the abrasive dispersion supply pipe 6 is pushed out and replaced with the TMAH liquid 85. The pure water and the TMAH liquid 85 flow out from the supply pipe 66 to the receiving container 104.

  At the stage where the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 are replaced with the TMAH liquid 85, the on-off valve 87 is closed to stop the supply of the TMAH liquid 85, and the slurry supply line 80, The TMAH liquid 85 is retained and held in the abrasive dispersion supply line 67 and the supply pipe 66 for a predetermined time (for example, 5 to 10 minutes). At this time, in the process in which the TMAH solution 85 which is an organic strong alkaline substance is in contact with the microorganisms attached and propagated on the inner wall of the slurry supply line 80, the abrasive dispersion supply line 67 and the supply pipe 66, the cells of the microorganisms are removed. Dissolve and sterilize. As a result, the TMAH solution 85, which is an organic strong alkali substance, sufficiently contacts and penetrates the microorganisms that adhere to and propagate on the inner wall of the supply line having the bent portion and are partially agglomerated. Cells can be lysed and sterilized. Further, the microorganisms are negatively charged due to the change of pH to the alkali side due to the supply of the TMAH liquid, and due to the electrical repulsive action between the slurry supply line 80 made of the abrasive resin material, the particle dispersion supply line 67, and the inner wall of the supply pipe 66. There is also physical detachment of microorganisms. The TMAH liquid 85 is not particularly limited, but is used after being diluted with ultrapure water to a concentration of 25%. It is used as the mainstream of developer in semiconductor factories and can be shared as a whole semiconductor manufacturing facility.

  As described above, by discharging the abrasive dispersion 2 from the abrasive dispersion supply line 7 and the abrasive dispersion supply pipe 6 and cleaning with pure water, the abrasive dispersion supply line 7, the abrasive The components of the abrasive dispersion 2 are removed from the surface of the microorganisms that have adhered and propagated on the inner wall and the inner wall of the particle dispersion supply pipe 6, and the TMAH solution 39 directly contacts and penetrates the microorganisms. Can be dissolved and sterilized.

  The pure water in the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 is extruded by supplying the TMAH liquid 85 and replaced with the TMAH liquid 85. The pure water in the supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 may be discharged, and then the TMAH liquid 85 may be supplied.

  FIG. 14 shows the state of the third step during cleaning for discharging the TMAH liquid 85 in the slurry supply line 80 and the abrasive dispersion supply line 67 by supplying nitrogen gas. In FIG. The same parts are denoted by the same reference numerals and the description thereof is omitted. In addition, the broken line arrow in a figure shows the flow of nitrogen gas. After retaining the TMAH solution 85 in the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 for a predetermined time, the on-off valve 87 is closed and the on-off valve 89 and the on-off valve 69 are opened. . The three-way switching valves 91, 92, 81 control the flow path in the nitrogen gas flow direction shown in FIG. Nitrogen gas is supplied from the nitrogen gas supply line 86 into the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 through the on-off valve 89, the three-way switching valves 91, 92, 81, and the cleaning liquid supply line 93. To do. As a result, the TMAH liquid 85 staying in the cleaning liquid supply line 93, the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 is discharged to the receiving container 104 through the opening / closing valve 69 and the flow meter 68.

  FIG. 15 shows a state of the fourth step at the time of cleaning in which the hydrogen peroxide solution is supplied into the slurry supply line 80 and the abrasive dispersion supply line 67. In FIG. 15, the same parts as those in FIGS. The same number is attached and explanation is omitted. The difference from FIGS. 11 and 15 is that the receiving container 105 that receives the hydrogen peroxide solution discharged from the supply pipe 66 is positioned. In the figure, solid arrows indicate the flow of hydrogen peroxide water, and broken arrows indicate the flow of nitrogen gas.

As described above, a predetermined amount of hydrogen peroxide solution (H ₂ O ₂ ) 95 is stored in the hydrogen peroxide solution container 94, and the hydrogen peroxide solution supply line 96 opened in the hydrogen peroxide solution container 94 has three sides. It is connected to a three-way switching valve 81 through switching valves 91 and 92 and a cleaning liquid supply line 93. At this time, the opening / closing valve 69 is opened, the opening / closing valve 100 related to the flow path of the hydrogen peroxide solution 95 is closed, and each of the three-way switching valves 91, 92, 81 flows in the direction indicated by the solid line arrow in the figure. The road is controlled.

  The on-off valve 98 is opened from the nitrogen gas supply line 97, and the supply pressure of nitrogen gas is applied to the upper surface of the hydrogen peroxide solution 95 in the hydrogen peroxide solution container 94. The hydrogen peroxide solution 95 in the hydrogen peroxide solution container 94 is pushed out to the hydrogen peroxide solution supply line 96, and the slurry supply line 80 is passed through the three-way switching valves 91 and 92, the cleaning liquid supply line 93, and the three-way switching valve 81. , Flows into the abrasive dispersion supply line 67 and the supply pipe 66. Further, it flows out from the supply pipe 66 to the receiving container 105 through the on-off valve 69 and the flow meter 68.

  When the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 are filled with the hydrogen peroxide solution 95, the on-off valve 98 is closed to stop the supply of the hydrogen peroxide solution 95 and the slurry. The hydrogen peroxide solution 95 is retained and held in the supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 for a predetermined time (for example, 5 to 10 minutes). At this time, the slurry supply line 80, the abrasive dispersion supply line 67, the inner wall of the supply pipe 66, the TMAH liquid 85, which is a strong alkali substance that remains attached to microorganisms, and the hydrogen peroxide solution 95 react to fire, thereby Separation of the microorganisms dissolved by the TMAH solution 85 from the inner walls of the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 and sterilization of the inner walls of the supply line can be further promoted.

  FIG. 16 shows the state of the fifth step during cleaning, which is a state in which the hydrogen peroxide solution 95 in the slurry supply line 80 and the abrasive dispersion supply line 67 by pure water supply is discharged. The same parts as those in FIGS. 11 and 15 are denoted by the same reference numerals, and the description thereof is omitted. In addition, the solid line arrow in a figure shows the flow of pure water.

  Pure water is supplied from the pure water supply line 101 into the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 through the open / close valve 102, the three-way switching valve 92, and the cleaning liquid supply line 93. Pure water flows through an on-off valve 69, a flow meter 68, and a supply pipe 66 with the slurry supply line 80 and the abrasive dispersion supply line 67 open, and is discharged to the receiving container 105 and supplied with the abrasive dispersion. The inside of the line 7 and the abrasive dispersion supply pipe 6 is cleaned with pure water. When pure water is allowed to flow out from the supply pipe 66 into the receiving container 105, the on-off valve 102 is closed to stop the supply of pure water. At this time, each of the related three-way switching valves 92 and 81 controls the flow path in the direction indicated by the solid line arrow in the figure. Thereby, the microorganisms adhering to the inner walls of the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 are discharged together with the hydrogen peroxide solution 95 and the pure water into the receiving container 105.

  FIG. 17 shows the state of the sixth step during cleaning in which pure water in the slurry supply line 80, abrasive dispersion supply line 67, and supply pipe 66 by nitrogen gas supply is discharged. , 16 are denoted by the same reference numerals and description thereof is omitted. In addition, the broken line arrow in a figure shows the flow of nitrogen gas.

  After the hydrogen peroxide solution 95 in the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66 is discharged and washed with pure water, the open / close valve 87 is closed and the open / close valve 69 is opened. The three-way switching valves 91, 92, 81 control the flow path in the nitrogen gas flow direction shown in FIG. The nitrogen gas is supplied from the nitrogen gas supply line 86 to the branch line 88, the on-off valve 89, the three-way switching valves 91, 92, 81, and the cleaning liquid supply line 93, and then to the slurry supply line 80, abrasive dispersion supply line 67, and supply pipe 66. Supply in. As a result, pure water is discharged into the receiving container 105.

  The microorganism removal and cleaning operations are completed by the first to sixth steps. The abrasive dispersion container 61 for storing the abrasive dispersion 62 again is mounted on the detachable member 65, and the slurry is produced and supplied to the polishing apparatus 83 as shown in FIG.

  In the embodiment, each on-off valve, three-way switching valve, and pump constituting the slurry supply device are individually controlled by a controller (not shown). Further, the abrasive dispersion liquid 62, the hydrogen peroxide solutions 72 and 95, and the TMAH liquid 85 are supplied by means of pressurizing with nitrogen gas, but supply means using a pump, a drop pressure, or the like may be used. Furthermore, the number of polishing stock solutions for slurry, the components, and the configuration of the slurry supply device are merely examples, and the present invention is not limited thereto. In addition to the slurry supply line 80, the abrasive dispersion supply line 67, and the supply pipe 66, the mixer 70 and the flow meter 68 can be cleaned simultaneously.

  In the second embodiment, the slurry supply line 80, the abrasive dispersion supply line 67, and the microorganisms attached to the supply pipe 66 are removed and cleaned. Also in each part and path of each of the slurry supply line 80, the abrasive dispersion supply line 67, and the mixer 70, which are at least part of the slurry that is a mixed liquid of the polishing stock solution to the supply line to the polishing apparatus. The basic microorganism removal and cleaning operations in the first to sixth steps may be performed individually.

  Further, the TMAH liquid 39, the hydrogen peroxide solution 50, the pure water, and the nitrogen gas are supplied from the three-way switching valve 81 provided in the slurry supply line 80, but the slurry is discharged to the polishing device 83 of the slurry supply line 80. You may make it supply from an exit. Further, in the cleaning step, the TMAH solution 85, the hydrogen peroxide solution 95, pure water, and nitrogen gas are supplied from the slurry supply line 80 and the abrasive dispersion supply line 7 in the opposite direction (reverse direction) to the flow of the slurry and the abrasive dispersion liquid 62. The supply pipe 66 is supplied and flowed, but it may be in the same direction. The abrasive dispersion container 61 is replaced with a new abrasive dispersion container 61 containing the abrasive dispersion 62 via the detachable member 65 when the abrasive dispersion 62 becomes empty. Therefore, at the time of cleaning, the containers 103, 104, and 105 that receive the abrasive dispersion liquid 62, the TMAH liquid 85, the hydrogen peroxide solution 95, and the pure water are also replaced through the detachable member 65 in the same manner as the abrasive dispersion container 61. Therefore, the TMAH solution 85, the hydrogen peroxide solution 95, the pure water, and the nitrogen gas are supplied from the abrasive dispersion 62 and the slurry supply line in the opposite direction (reverse direction) to the slurry flow. 80, and preferably supplied to the abrasive dispersion supply line 67 and the supply pipe 66 to flow.

  In the second embodiment, the polishing apparatus 83 is stopped during cleaning, but the cleaning may be performed during regular maintenance of the slurry supply apparatus or the polishing apparatus 83. In addition, by providing two slurry supply devices for one polishing layer device 83, cleaning can be performed without stopping the polishing layer device 83.

  Next, another configuration of the second embodiment will be described with reference to FIG. This is a microbe detection apparatus that removes the polishing stock solution or slurry from a plurality of sites from a supply line of the polishing stock solution to a supply line of slurry that is a mixed liquid of the plurality of polishing stock solutions. The configuration and operation will be described with reference to FIG. 18. The same reference numerals as those in FIG.

  A detection line 67 a branched from the abrasive dispersion supply line 67 is connected to the switching valve 400, and further, the switching valve 400 and the microorganism detection device 200 are connected via the detection line 203. The sterilizing means 300 is provided on the downstream side of the abrasive dispersion supply line 67 from which the detection line 67a is branched.

  Further, the detection line 82 a branched from the slurry discharge line 82 is connected to the switching valve 400, and the switching valve 400 and the microorganism detection device 200 are connected to each other via the detection line 203. The sterilizing means 300 is provided on the downstream side of the circulation line 24 where the detection line 82a is branched.

  In the above-described configuration, the flow path is switched by the switching valve 400 so that the abrasive dispersion 62 from the abrasive dispersion supply line 67 and the slurry from the slurry discharge line 82 are sequentially led to the microorganism detection apparatus 200. The operations of the microorganism detecting apparatus 200 and the sterilizing means 300 are the same as those described above, and the description thereof is omitted.

  Thus, in the supply line from the polishing stock solution supply line to the polishing apparatus for the slurry, which is a mixed liquid of the plurality of polishing stock solutions, the number of microorganism detection devices is reduced and the site where microorganisms are present or the breeding site is specified. Can do. As described above, also in the second embodiment, the same effects as in the first embodiment can be obtained.

  In Examples 1 and 2, the microorganism detection apparatus is described as an example of using the slurry supply apparatus. However, the present invention is not limited to this, and microorganisms are not contained in the liquid to be measured in which microorganisms and solid particles other than microorganisms exist. The present invention can be applied to various fields that need to be detected. For example, sludge treatment equipment in the environmental field, and analysis of cleaning liquid in the food field.

  The present invention can also be applied to a wide range of apparatuses that require detection of microorganisms in a liquid to be measured.

Basic configuration diagram of slurry supply apparatus of embodiment 1 of the present invention Basic configuration diagram of microorganism detection means The graph which shows the example of the output signal from the light-receiving part of a microbe detection apparatus The block diagram of the slurry supply apparatus which shows the state of the 1st step at the time of the washing | cleaning which discharges the abrasive grain dispersion liquid by a pure water supply The block diagram of the slurry supply apparatus which shows the state of the 2nd step at the time of the washing | cleaning which supplies a TMAH liquid The block diagram of the slurry supply apparatus which shows the state of the 3rd step at the time of the washing | cleaning which discharges the TMAH liquid by nitrogen gas supply The block diagram of the slurry supply apparatus which shows the state of the 4th step at the time of the washing | cleaning which supplies hydrogen peroxide water The block diagram of the slurry supply apparatus which shows the state of the 5th step at the time of the washing | cleaning which discharges the hydrogen peroxide solution by a pure water supply The block diagram of the slurry supply apparatus which shows the state of the 6th step at the time of the washing | cleaning which discharges the pure water by nitrogen gas supply The figure which shows the other structure of Example 1. Basic configuration diagram of slurry supply apparatus of embodiment 2 of the present invention The block diagram of the slurry supply apparatus which shows the state of the 1st step at the time of the washing | cleaning which discharges the abrasive grain dispersion liquid by a pure water supply The block diagram of the slurry supply apparatus which shows the state of the 2nd step at the time of the washing | cleaning which supplies a TMAH liquid The block diagram of the slurry supply apparatus which shows the state of the 3rd step at the time of the washing | cleaning which discharges the TMAH liquid by nitrogen gas supply The block diagram of the slurry supply apparatus which shows the state of the 4th step at the time of the washing | cleaning which supplies hydrogen peroxide water The block diagram of the slurry supply apparatus which shows the state of the 5th step at the time of the washing | cleaning which discharges the hydrogen peroxide solution by a pure water supply The block diagram of the slurry supply apparatus which shows the state of the 6th step at the time of the washing | cleaning which discharges the pure water by nitrogen gas supply The figure which shows the other structure of Example 2.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Abrasive dispersion container 2 Abrasive dispersion 3 Nitrogen gas supply line 4 On-off valve 5 Detachable member 6 Abrasive dispersion supply pipe 7 Abrasive dispersion supply line 7a Detection line 8 Open / close valve 9 Bending part 10 Three-way switching valve 11 Slurry mixed storage container 12 Slurry (mixed polishing liquid)
13 Hydrogen peroxide solution container 14 Hydrogen peroxide solution 15 Nitrogen gas supply line 16 Open / close valve 17 Detachable member 18 Supply pipe 19 Hydrogen peroxide solution supply line 20 Open / close valve 21 Pure water supply line 22 Pure water branch line 23 Open / close valve 24 Circulation Line 24a Detection line 25 Pump 26 Slurry supply line 27 Open / close valve 28 Slurry mixing and storage container 29 Slurry 30 Circulation line 30a Detection line 31 Pump 32 Slurry supply line 33 Pump 34 Polishing device 35 Slurry supply line 36 Pump 37 Polishing device 38 TMAH liquid container 39 TMAH liquid 40 TMAH liquid supply line 41 Three-way switching valve 42 Open / close valve 43 Three-way switching valve 44 Cleaning liquid supply line 45 Nitrogen gas supply line 46 Open / close valve 47 Branch line 48 Open / close valve 49 Hydrogen peroxide solution container 50 Hydrogen peroxide solution 51 Hydrogen peroxide water supply line 52 Nitrogen gas supply line 53 On-off valve 54 Branch line 55 On-off valve 56 Branch line 57 On-off valve 58 Receiving container 59 Receiving container 60 Receiving container 61 Abrasive dispersion liquid container 62 Abrasive dispersion liquid 63 Nitrogen gas Supply line 64 On-off valve 65 Detachable member 66 Supply pipe (Abrasive dispersion supply line)
67 Abrasive dispersion supply line 68 Flow meter 69 On-off valve 70 Mixer 71 Hydrogen peroxide solution container 72 Hydrogen peroxide solution 73 Nitrogen gas supply line 74 On-off valve 75 Detachable member 76 Supply pipe 77 Hydrogen peroxide solution supply line 78 Flow rate Total 79 Open / close valve 80 Slurry supply line 81 Three-way switching valve 82 Slurry discharge line 83 Polishing device 84 TMAH liquid container 85 TMAH liquid 86 Nitrogen gas supply line 87 Open / close valve 88 Branch line 89 Open / close valve 90 Supply pipe 91 Three-way switch valve 92 Three-way switch Valve 93 Cleaning liquid supply line 94 Hydrogen peroxide solution container 95 Hydrogen peroxide solution 96 Hydrogen peroxide solution supply line 97 Nitrogen gas supply line 98 On-off valve 99 Branch line 100 On-off valve 101 Pure water supply line 102 On-off valve 103 Receiving vessel 104 Receiving vessel Container 105 Receiving container 200 Microbiological test Outlet device 201 Tubing body 201a Pipe line 202 Connection member 203 Detection line 204 Light emitting unit 205 Light receiving unit 206 Arithmetic unit 207 Controller 208 Notifying unit 300 Sterilizing unit 400 Switching valve

Claims (13)

The liquid to be measured containing abrasive grains is irradiated with light of first and second different wavelengths, the light of the first wavelength is ultraviolet, the light of the second wavelength is infrared, and the first The difference between the transmission amount of the abrasive grains, which are solids other than microorganisms, and the solid matter other than the microorganisms, by the light at the wavelength, and the transmission amount of the abrasive grains, which is solid matter other than the microorganisms, at the second wavelength, A method for detecting a microorganism, comprising detecting the presence. The test liquid flowing was tube body containing abrasive grains, a first light emitting unit for irradiating light having a wavelength of, prior Symbol solids other than the transmission amount and the microorganism of microorganisms light of the first wavelength is ultraviolet a light receiving portion for detecting a permeation amount of the abrasive grains is, the on target solution, a light emitting unit for emitting light of the second wavelength is an infrared, solid non microorganisms before Symbol second wavelength light A light receiving unit that detects the amount of transmission of the abrasive grains that are objects, the amount of transmission of the abrasive grains that are solids other than microorganisms and microorganisms by irradiation with light of the first wavelength, and light of the second wavelength And a calculation means for calculating a difference between the amount of the abrasive grains that are solids other than the microorganisms by the irradiation, and detecting the presence of the microorganism based on the difference in the transmission amount calculated by the calculation means. Microbe detection device. The microorganism detection apparatus according to claim 2, wherein the permeation amount is an integrated value in a predetermined amount of fluid to be measured that flows. The microorganism detection apparatus according to claim 2 or 3, wherein a transmission amount of light having the first wavelength and light having the second wavelength is measured with a spectrum analyzer. The microorganism detection apparatus according to any one of claims 2 to 4, further comprising an informing means for informing the presence of microorganisms. Microorganism detection according to any one of claims 2-5 for detecting any site microorganisms leading to the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock The slurry supply apparatus provided with the apparatus. To multiple sites leading to the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock, a slurry supply according to claim 6, comprising the microorganism detection apparatus apparatus. Claim that a plurality of portions extending in the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock, the grinding stock solution or slurry, characterized in that to derive the microorganism detection apparatus 6. The slurry supply apparatus according to 6. At least a portion of the site leading to the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock, comprising a sterilizing unit for sterilizing microorganisms, the number of detection by the microorganism detecting device The slurry supply apparatus according to any one of claims 6 to 8, wherein the sterilizing means is driven on the basis of the above. Comprising a cleaning means for cleaning at least a portion of the site leading to the supply line from the supply line of polishing stock solution to the polishing apparatus of the slurry is a mixture before Symbol Migaku Ken stock, based on the detection value of the number of microorganisms according to the microorganism detection apparatus 10. At least a part of the polishing stock solution from the supply line of the polishing stock solution to the supply line of the slurry, which is a mixed solution of the plurality of polishing stock solutions, to the polishing apparatus is washed. The slurry supply apparatus according to item. After at least a portion of the supply line leading to the polishing apparatus of the slurry is a mixed grinding stock prior Symbol Migaku Ken stock from the supply line of polishing stock supplies a tetramethylammonium hydroxide (TMAH) solution discharge, hydrogen peroxide The slurry supply apparatus according to claim 10, wherein water is supplied and discharged. The slurry supply apparatus according to claim 11, wherein an aqueous tetramethylammonium hydroxide solution is supplied and retained in a supply line for a predetermined time. The slurry supply apparatus according to claim 11 or 12, wherein hydrogen peroxide water is supplied and retained in a supply line for a predetermined time.

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