QUALITY INSPECTION METHOD FOR CHEMICAL LIQUID

• US 20190324373A1
• Filed: 07/03/2019
• Published: 10/24/2019
• Est. Priority Date: 01/06/2017
• Status: Active Grant

• Current Assignee: Fujifilm Corporation (Fujifilm Holdings Corporation)
• Original Assignee: Fujifilm Corporation (Fujifilm Holdings Corporation)
• Inventors: KAMIMURA, Tetsuya
• Granted Patent: US 11,392,046 B2
• Time in Patent Office: Days
• CPC Class Codes: G01N 2001/386 Other diluting or mixing processes
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 2030/027 Liquid chromatography
• CPC Class Codes: G01N 21/3103 Atomic absorption analysis
• CPC Class Codes: G01N 24/08 by using nuclear magnetic resonance G01N24/12 takes precedence
• CPC Class Codes: G01N 30/06 Preparation
• CPC Class Codes: G01N 30/7206 interfaced to gas chromatograph interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04
• CPC Class Codes: G01N 30/7233 interfaced to liquid or supercritical fluid chromatograph interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04
• CPC Class Codes: G01N 33/2028 Metallic constituents
• CPC Class Codes: G01N 33/442 Resins; Plastics
• CPC Class Codes: G03F 7/26 Processing photosensitive materials; Apparatus therefor G03F7/12 - G03F7/24 take precedence
• CPC Class Codes: G03F 7/7065 Defects, e.g. optical inspection of patterned layer for defects
• CPC Class Codes: H01L 21/027 Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 photographic masks or originals per se G03F1/00; registration or positioning of photographic masks or originals G03F9/00; photographic cameras G03B; control of position G05D3/00
• CPC Class Codes: H01L 21/304 Mechanical treatment, e.g. grinding, polishing, cutting H01L21/30625 takes precedence
• CPC Class Codes: H01L 22/10 Measuring as part of the manufacturing process burn-in G01R31/2855

Abstract

An object of the present invention is to provide a quality inspection method for a chemical liquid that makes it possible to simply evaluate defect performance.

The quality inspection method according to an embodiment of the present invention is a quality inspection method for a chemical liquid used for manufacturing a semiconductor substrate, including a step W of preparing a first container and washing at least a portion of a liquid contact portion by using a portion of the chemical liquid, a step A of performing concentration of a portion of the chemical liquid by using the washed first container so as to obtain c liquid, a step B of performing measurement of a content of a specific component in c liquid, and a step C of comparing the content of the specific component with a preset standard value. The step W, the step A, the step B, and the step C are performed in this order, at least the step W and the step A are performed in a clean room having cleanliness equal to or higher than class 4 specified in ISO14644-1:2015, the concentration is performed in at least one kind of inert gas selected from the group consisting of an Ar gas, a He gas, and a N₂ gas or under reduced pressure, and the measurement is performed by a predetermined measurement method.

Claims

1. A quality inspection method for a chemical liquid used for manufacturing a semiconductor substrate, comprising:

a step W of preparing a first container having a liquid contact portion of which at least a portion is formed of at least one kind of material selected from the group consisting of glass, a fluorine-containing polymer, and electropolished stainless steel, adopting a portion of the chemical liquid as a liquid, and washing at least a portion of the liquid contact portion by using a liquid;

a step A of adopting a portion of the chemical liquid as b liquid and performing concentration of b liquid by using the washed first container so as to obtain c liquid;

a step B of performing measurement of a content of a specific component in c liquid; and

a step C of comparing the content of the specific component with a preset standard value,

wherein the step W, the step A, the step B, and the step C are performed in this order,

at least the step W and the step A are performed in a clean room having cleanliness equal to or higher than class 4 specified in the International Standard ISO14644-1;

2015 established by the International Organization for Standardization,

the concentration is performed under at least one kind of inert gas selected from the group consisting of an Ar gas, a He gas, and a N₂ gas or under reduced pressure, and

the measurement is performed by at least one kind of measurement method selected from the group consisting of gas chromatography mass spectrometry, gas chromatography tandem mass spectrometry, gas chromatography atomic emission detection, gas chromatography quadrupole time-of-flight type mass spectrometry, direct sample introduction-type mass spectrometry, high-performance liquid chromatography mass spectrometry, high-performance liquid chromatography tandem mass spectrometry, high-performance liquid chromatography time-of-flight type mass spectrometry, inductively coupled plasma mass spectrometry, inductively coupled plasma emission spectrometry, temperature programmed desorption mass spectrometry, ion chromatography, nuclear magnetic resonance spectrometry, and atomic absorption spectrometry.

2. The quality inspection method for a chemical liquid according to claim 1, further comprising:

a step D of determining the chemical liquid as being inadequate and discarding the chemical liquid in a case where the content of the specific component is greater than the standard value in the step C;

or

a step E of purifying the chemical liquid in a case where the content of the specific component is greater than the standard value in the step C and then performing again the step W, the step A, the step B, and the step C.

3. The quality inspection method for a chemical liquid according to claim 1,

wherein the step B is also performed in the clean room.

4. The quality inspection method for a chemical liquid according to claim 1,

wherein the step W further has at least one kind of step selected from the group consisting of a step of performing acid washing on at least the liquid contact portion of the first container, a step of performing ultrasonic washing on at least the liquid contact portion of the first container, and a step of drying at least the liquid contact portion of the first container.

5. The quality inspection method for a chemical liquid according to claim 1,

wherein a factor of concentration in the step A is 2 to 1,000,000.

6. The quality inspection method for a chemical liquid according to claim 1,

wherein a factor of concentration in the step A is 10 to 10,000.

7. The quality inspection method for a chemical liquid according to claim 1,

wherein the specific component contains at least one kind of compound selected from the group consisting of Formulae (1) to (7).

8. The quality inspection method for a chemical liquid according to claim 1,

wherein a temperature condition of the concentration in the step A is 10°

C. to 250°

C.

9. The quality inspection method for a chemical liquid according to claim 1,

wherein a volume of b liquid in the step A is equal to or smaller than 5 L.

10. The quality inspection method for a chemical liquid according to claim 1,

wherein in a case where the first container is a fluorine-containing polymer container in which at least a portion of the liquid contact portion is formed of a fluorine-containing polymer, the fluorine-containing polymer container satisfies a condition 1 or a condition 2 in the following test,

test:

a portion of the chemical liquid is adopted as d liquid, the liquid contact portion is washed using d liquid, a portion of the chemical liquid is adopted as e liquid, and under the condition that a ratio of a mass of the washed fluorine-containing polymer container to a mass of e liquid becomes 1.0 provided that a liquid temperature of e liquid is 25°

C., the washed fluorine-containing polymer container is immersed for 24 hours in e liquid having a liquid temperature of 25°

C.,

condition 1;

in a case where e liquid having been used for the immersion contains one kind of fluoride ion, an increase of one kind of the fluoride ion before and after the immersion is equal to or smaller than 1 mass ppm,

condition 2;

in a case where e liquid having been used for the immersion contains two or more kinds of fluoride ions, a total increase of two or more kinds of the fluoride ions before and after the immersion is equal to or smaller than 1 mass ppm.

11. The quality inspection method for a chemical liquid according to claim 1,

wherein in a case where the first container is a fluorine-containing polymer container in which at least a portion of the liquid contact portion is formed of a fluorine-containing polymer, within a surface of at least a portion of the liquid contact portion, provided that an atom number ratio of the number of fluorine atoms contained in the surface to the number of carbon atoms contained in the surface is M₁, and an atom number ratio of the number of fluorine atoms contained in a position, which is 10 nm below the surface in a thickness direction of the fluorine-containing polymer container, to the number of carbon atoms contained in the position is M_2, a ratio of M₁ to M₂ is higher than 1.0.

12. The quality inspection method for a chemical liquid according to claim 1,

wherein in a case where the first container is an electropolished stainless steel container in which at least a portion of the liquid contact portion is formed of electropolished stainless steel, the electropolished stainless steel container satisfies a condition 3 or a condition 4 in the following test,

test:

a portion of the chemical liquid is adopted as f liquid, the liquid contact portion is washed using f liquid, a portion of the chemical liquid is adopted as g liquid, and under the condition that a ratio of a mass of the washed electropolished stainless steel container to a mass of g liquid becomes 0.25 provided that a liquid temperature of g liquid is 25°

C., the washed electropolished stainless steel container is immersed for 24 hours in g liquid having a liquid temperature of 25°

C.,

condition 3;

in a case where g liquid having been used for the immersion contains one kind of metal component, an increase of one kind of the metal component before and after the immersion is equal to or smaller than 1 mass ppm,

condition 4;

in a case where g liquid having been used for the immersion contains two or more kinds of metal components, a total increase of two or more kinds of the metal components before and after the immersion is equal to or smaller than 1 mass ppm.

13. The quality inspection method for a chemical liquid according to claim 1,

wherein in a case where the first container is an electropolished stainless steel container in which at least a portion of the liquid contact portion is formed of electropolished stainless steel, within a surface of at least a portion of the liquid contact portion, provided that an atom number ratio of the number of chromium atoms contained in the surface to the number of iron atoms contained in the surface is P₁, and an atom number ratio of the number of chromium atoms contained in a position, which is 10 nm below the surface in a thickness direction of the electropolished stainless steel container, to the number of iron atoms contained in the position is P₂, a ratio of P₁ to P₂ is higher than 1.0.

14. The quality inspection method for a chemical liquid according to claim 1,

wherein in a case where the first container is an electropolished stainless steel container in which at least a portion of the liquid contact portion is formed of electropolished stainless steel, within a surface of at least a portion of the liquid contact portion, an atom number ratio of the number of chromium atoms contained in a position, which is 1 nm below the surface in a thickness direction of the electropolished stainless steel container, to the number of iron atoms contained in the position is equal to or higher than 1.0.

15. The quality inspection method for a chemical liquid according to claim 1,

wherein the chemical liquid contains at least one kind of organic solvent selected from the group consisting of propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monopropyl ether, propylene glycol monomethyl ether acetate, ethyl lactate, methoxymethyl propionate, cyclopentanone, cyclohexanone, γ

-butyrolactone, diisoamyl ether, butyl acetate, isoamyl acetate, isopropanol, and 4-methyl-2-pentanol.

16. The quality inspection method for a chemical liquid according to claim 1,

wherein the measurement includes organic analysis for measuring a content of an organic component in c liquid and inorganic analysis for measuring a content of an inorganic component in c liquid.

17. The quality inspection method for a chemical liquid according to claim 1,

wherein the measurement is performed by at least one kind of measurement method selected from the group consisting of gas chromatography mass spectrometry, gas chromatography tandem mass spectrometry, high-performance liquid chromatography mass spectrometry, high-performance liquid chromatography tandem mass spectrometry, and inductively coupled plasma mass spectrometry.

18. The quality inspection method for a chemical liquid according to claim 1,

wherein the measurement is performed by at least one kind of measurement method selected from the group consisting of high-performance liquid chromatography mass spectrometry and high-performance liquid chromatography tandem mass spectrometry.

19. The quality inspection method for a chemical liquid according to claim 1,

wherein each of the content of the specific component measured in the step B and the standard value compared in the step C is an absolute quantity.

20. The quality inspection method for a chemical liquid according to claim 1,

wherein each of the content of the specific component measured in the step B and the standard value compared in the step C is a relative quantity.

21. The quality inspection method for a chemical liquid according to claim 1,

wherein the specific component contains an organic substance having a boiling point equal to or higher than 200°

C.

22. The quality inspection method for a chemical liquid according to claim 21, wherein the specific component contains an organic substance having a boiling point of 300°

C. to 800°

C.

23. The quality inspection method for a chemical liquid according to claim 1,

wherein the specific component contains an organic substance having a molecular weight equal to or greater than 200.

24. The quality inspection method for a chemical liquid according to claim 23,

wherein the specific component contains an organic substance having a molecular weight of 300 to 1,000.

25. The quality inspection method for a chemical liquid according to claim 1,

wherein the measurement is performed by at least one kind of measurement method selected from the group consisting of gas chromatography mass spectrometry, gas chromatography tandem mass spectrometry, high-performance liquid chromatography mass spectrometry, and high-performance liquid chromatography tandem mass spectrometry, and

the specific component contains an organic substance in which m/Z is 300 to 1,000.

26. The quality inspection method for a chemical liquid according to claim 1, further comprising:

a specific component determination step that is performed before the step W or between the step W and the step A,

wherein the specific component determination step includes a step W3 of preparing a third container having a liquid contact portion of which at least a portion is formed of at least one kind of material selected from the group consisting of glass, a fluorine-containing polymer, and electropolished stainless steel, adopting a portion of the chemical liquid as h liquid, and washing at least a portion of the liquid contact portion of the third container by using h liquid, a step A3 of adopting a portion of the chemical liquid as i liquid and concentrating i liquid by using the washed third container so as to obtain three or more kinds of j liquids having different factors of concentration, a step B3 of performing measurement of a content of an organic substance, in which m/Z is 300 to 1,000, in j liquids by at least one kind of measurement method selected from the group consisting of high-performance liquid chromatography mass spectrometry and gas chromatography mass spectrometry, and a step C3 in which in a case where one kind of organic substance is commonly detected from all of three or more kinds of j liquids, one kind of the organic substance is determined as a specific component, and in a case where two or more kinds of organic substances are commonly detected from all of three or more kinds of j liquids, from a coefficient of correlation obtained by performing linear regression on the factors of concentration and the content of each of two or more kinds of the organic substances and a coefficient of correlation obtained by performing linear regression on the factors of concentration and the total content of organic substances in a combination of two or more kinds of the organic substances, a maximum coefficient of correlation is selected, and an organic substance or a combination of organic substances from which the maximum coefficient of correlation is obtained is determined as a specific component, the step W3, the step A3, the step B3, and the step C3 are performed in this order, at least the step W3 and the step A3 are performed in a clean room having cleanliness equal to or higher than class 4 specified in the International Standard ISO14644-1;

2015 established by the International Organization for Standardization, and

the concentration of i liquid is performed under at least one kind of inert gas selected from the group consisting of an Ar gas, a He gas, and a N₂ gas or under reduced pressure.

27. The quality inspection method for a chemical liquid according to claim 26, further comprising:

a standard value determination step of determining the standard value at a point in time when the specific component determination step has finished but the step C is not yet started,

wherein the standard value determination step includes a step W4 of preparing n pieces of fourth containers each having a liquid contact portion of which at least a portion is formed of at least one kind of material selected from the group consisting of glass, a fluorine-containing polymer, and electropolished stainless steel, preparing n kinds of chemical liquids manufactured by different manufacturing methods, obtaining twice a portion of each of n kinds of the chemical liquids, naming the obtained chemical liquids as p₁ liquid and p₂ liquid respectively, and washing at least a portion of the liquid contact portion of each of the fourth containers by using each of p₁ liquids, a step A4 of performing concentration of each of the corresponding liquids p₂ by using each of the fourth containers washed with each of the liquids p₁ so as to obtain n kinds of liquids q, a step B4 of performing measurement of a content of a specific component in each of q liquids by at least one kind of measurement method selected from the group consisting of high-performance liquid chromatography mass spectrometry and gas chromatography mass spectrometry, a step S of evaluating a defect inhibition performance of each of n kinds of the chemical liquids by using a defect inspection device, a step T of creating a calibration curve by performing linear regression on the content of the specific component and the defect inhibition performance, and a step U of determining the content of the specific component corresponding to a predetermined defect inhibition performance as a standard value by using the calibration curve,

the step W4, the step A4, the step B4, the step S, the step T, and the step U are performed in this order,

at least the step W4 and the step A4 are performed in a clean room having cleanliness equal to or higher than class 4 specified in the International Standard ISO14644-1;

2015 established by the International Organization for Standardization,

the concentration of p₂ liquid is performed under at least one kind of inert gas selected from the group consisting of an Ar gas, a He gas, and a N₂ gas or under reduced pressure, and

n represents an integer equal to or greater than 3.

28. The quality inspection method for a chemical liquid according to claim 1,

wherein the measurement includes inorganic analysis for analyzing a content of an inorganic component in c liquid, and

provided that the content of the specific component measured in the step B is an absolute quantity, the absolute quantity is determined by a standard addition method.

29. The quality inspection method for a chemical liquid according to claim 1,

wherein the measurement includes inorganic analysis for measuring a content of an inorganic substance in c liquid, and

the inorganic analysis is measurement of a content of at least 5 or more kinds of atoms selected from the group consisting of Ag, Al, As, Au, Ba, Ca, Cd, Co, Cr, Cu, Fe, Ga, Ge, K, Li, Mg, Mn, Mo, Na, Nb, Ni, Pb, Sb, Sn, Sr, Ta, Th, Ti, Tl, V, W, Zn, and Zr in c liquid.

30. The quality inspection method for a chemical liquid according to claim 29,

wherein 5 or more kinds of the atoms contain at least two or more kinds of atoms selected from the group consisting of Al, Fe, and Ti.

31. The quality inspection method for a chemical liquid according to claim 1,

wherein in a case where the content of the specific component is be equal to or smaller than the standard value in the step C, the chemical liquid is determined as being adequate.