WO2024034797A1 - Film-type color-sensing device for detecting volatile basic nitrogen gas and manufacturing method therefor - Google Patents
Film-type color-sensing device for detecting volatile basic nitrogen gas and manufacturing method therefor Download PDFInfo
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- WO2024034797A1 WO2024034797A1 PCT/KR2023/007329 KR2023007329W WO2024034797A1 WO 2024034797 A1 WO2024034797 A1 WO 2024034797A1 KR 2023007329 W KR2023007329 W KR 2023007329W WO 2024034797 A1 WO2024034797 A1 WO 2024034797A1
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- color
- film
- pdms
- basic nitrogen
- nitrogen gas
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910001873 dinitrogen Inorganic materials 0.000 title claims abstract description 49
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 79
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 79
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- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract 29
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract 29
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 33
- 238000001514 detection method Methods 0.000 claims description 29
- BELBBZDIHDAJOR-UHFFFAOYSA-N Phenolsulfonephthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2S(=O)(=O)O1 BELBBZDIHDAJOR-UHFFFAOYSA-N 0.000 claims description 25
- 229960003531 phenolsulfonphthalein Drugs 0.000 claims description 25
- 239000011241 protective layer Substances 0.000 claims description 20
- FRPHFZCDPYBUAU-UHFFFAOYSA-N Bromocresolgreen Chemical compound CC1=C(Br)C(O)=C(Br)C=C1C1(C=2C(=C(Br)C(O)=C(Br)C=2)C)C2=CC=CC=C2S(=O)(=O)O1 FRPHFZCDPYBUAU-UHFFFAOYSA-N 0.000 claims description 19
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- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 12
- 229940012189 methyl orange Drugs 0.000 claims description 12
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 claims description 12
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 12
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- ABIUHPWEYMSGSR-UHFFFAOYSA-N bromocresol purple Chemical compound BrC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(Br)C(O)=C(C)C=2)=C1 ABIUHPWEYMSGSR-UHFFFAOYSA-N 0.000 claims description 6
- NUHCTOLBWMJMLX-UHFFFAOYSA-N bromothymol blue Chemical compound BrC1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C(=C(Br)C(O)=C(C(C)C)C=2)C)=C1C NUHCTOLBWMJMLX-UHFFFAOYSA-N 0.000 claims description 6
- PGSADBUBUOPOJS-UHFFFAOYSA-N neutral red Chemical compound Cl.C1=C(C)C(N)=CC2=NC3=CC(N(C)C)=CC=C3N=C21 PGSADBUBUOPOJS-UHFFFAOYSA-N 0.000 claims description 6
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Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/80—Indicating pH value
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
Definitions
- the present invention relates to a film-type color sensing device for detecting volatile basic nitrogen gas and a method of manufacturing the same.
- ammonia is designated as a flammable, toxic and hazardous chemical in the 'High Pressure Gas Safety Management Act' and the 'Chemical Substances Control Act', but it is widely used in various industrial fields because of its excellent performance as a refrigerant.
- micro-leakage of ammonia may occur due to problems such as aging facilities, and cases of multiple casualties due to ammonia leakage accidents are frequently reported.
- the Occupational Safety and Health Administration limits the leakage of ammonia to less than 50ppm in an 8-hour workday. It is known that exposure to ammonia above this limit can cause a burning sensation in the eyes, nose, throat, and respiratory tract. .
- proteins are decomposed into amino acids by the enzymatic action of proliferating microorganisms (spoilage bacteria), and the amino acids are then changed into volatile amines through decarboxylation.
- TVBN Total Volatile Basic Nitrogen
- a sensor In the case of a sensor to be included in food packaging, it must have flexibility, adhesiveness, and be able to respond selectively to volatile amines without being affected by interfering substances such as moisture from meat and fish and shellfish, and allow users to easily know the freshness of food. do.
- the sensor manufacturing process must be relatively simple, large-scale, and easy to use and dispose of by workers and food purchasers in industrial sites, so a volatile base that can meet these requirements is needed.
- the development of sensors for nitrogen gas detection is required.
- a film-type color sensing device for detecting volatile basic nitrogen gas and a manufacturing method thereof according to an embodiment of the present invention were proposed to solve the above problems, and are easy for users to use, can be expanded to a large area at low cost, and are flexible.
- the purpose is to have high specificity for volatile basic nitrogen and ammonia gas.
- a color sensing unit includes a predetermined reactive dye so that a color change occurs in response to a basic gas, and is provided in the form of a layer with a predetermined thickness; A first polymer protection part laminated on one side of the color sensing part with the color sensing part in between, and made of PDMS material having hydrophobicity and gas permeability to transmit the basic gas and prevent leakage of the reactive dye; And a second polymer protection part laminated on the other side of the color sensing part with the color sensing part in between, and made of PDMS material having hydrophobicity and gas permeability to transmit the basic gas and prevent leakage of the reactive dye.
- a film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
- a film-type color sensing device for detecting volatile basic nitrogen gas may be provided, wherein the basic gas is volatile basic nitrogen.
- the reactive dyes are commercial pH indicator dyes, such as bromocresol green (BCG), phenol red (PR), methyl orange (MO), methyl red (MR), litmus, and methyle purple, which change color between pH 4 and 8.
- BCG bromocresol green
- PR phenol red
- MO methyl orange
- MR methyl red
- litmus methyle purple
- a film-type color detection device for detecting volatile basic nitrogen gas may be provided, characterized in that any one of (MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and universal indicator is used.
- the color sensing unit mixes the reactive dye with a PDMS solution in which PDMS and PDMS curing agent are mixed at a mass ratio of 10:1, performs spin coating, and then thermally cures it to form a flexible film with a thickness of 55 to 65 um.
- a film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
- first polymer protection part and the second polymer protection part are provided in the form of a flexible film with a thickness of 15 to 25 um through spin coating by mixing PDMS and PDMS curing agent at a mass ratio of 10:1 and heat curing.
- a film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
- a method of manufacturing a film-type color sensing device for gas detection can be provided.
- first polymer protection part and the second polymer protection part are manufactured to have a thickness of 15 to 25 um, and the color sensing part is manufactured to have a thickness of 55 to 65 um.
- a method of manufacturing a color sensing device may be provided.
- a color-sensing layer includes a predetermined reactive dye so that a color change occurs in response to a basic gas, and is provided in the form of a layer of a predetermined thickness on the surface of a food resin material; and a protective layer laminated on one side of the color sensing unit corresponding to the opposite side of the food resin material and made of PDMS material having hydrophobicity and gas permeability to transmit the basic gas and prevent leakage of the reactive dye.
- a film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
- a film-type color sensing device for detecting volatile basic nitrogen gas may be provided, wherein the basic gas is volatile basic nitrogen.
- the reactive dyes are commercial pH indicator dyes, such as bromocresol green (BCG), phenol red (PR), methyl orange (MO), methyl red (MR), litmus, and methyle purple, which change color between pH 4 and 8.
- BCG bromocresol green
- PR phenol red
- MO methyl orange
- MR methyl red
- litmus methyle purple
- a film-type color detection device for detecting volatile basic nitrogen gas may be provided, characterized in that any one of (MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and universal indicator is used.
- the color-sensing layer is created by mixing and stirring the reactive dye in the PDMS solution, diluting it with a hexane solution, applying it to the food resin material by spraying it, and then heat-treating it under predetermined conditions.
- a film-type color sensing device for detecting volatile basic nitrogen gas may be provided, characterized in that it is provided in the form of a coating layer.
- the color sensing layer is mixed with the reactive dye in the PDMS solution, stirred at 100 to 300 rpm for 22 to 26 hours, and diluted with a hexane solution, and then applied to the surface of the food resin material at a pressure of 35 to 45 psi.
- Film-type color detection for detecting volatile basic nitrogen gas characterized by spraying for 3 to 5 seconds through a 150 to 250um nozzle at a distance of 25 to 35 cm and heat treatment at 55 to 65 ° C for 1 to 3 minutes after application.
- a device may be provided.
- the protective layer is provided in the form of a coating layer surrounding the color-sensing layer by applying a PDMS solution mixed with PDMS and PDMS curing agent on the surface of the color-sensing layer through a spray method and then heat-treating it under predetermined conditions.
- a film-type color sensing device for detecting volatile basic nitrogen gas can be provided.
- the protective layer is spray-applied for 3 to 5 seconds at a distance of 25 to 35 cm from the surface of the color-sensing layer at a pressure of 35 to 45 psi, and heat treated at 55 to 65 ° C for 1 to 3 minutes after application.
- a film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
- mixing and stirring a reactive dye in a PDMS solution diluting it with a hexane solution, and spraying it on the surface of a food resin material at a predetermined pressure; Forming a color-sensitive layer in the form of a coating layer by heat-treating it under predetermined conditions after spray application; After the color-sensing layer is formed, applying a PDMS solution onto the surface of the color-sensing layer; and applying the PDMS solution and then heat-treating it under predetermined conditions to form a protective layer in the form of a coating layer surrounding the color-sensing layer.
- a method of manufacturing a film-type color sensing device for detecting volatile basic nitrogen gas will be provided, including You can.
- the color sensing layer is mixed with the reactive dye in the PDMS solution, stirred at 100 to 300 rpm for 22 to 26 hours, and diluted with a hexane solution, and then applied to the surface of the food resin material at a pressure of 35 to 45 psi.
- Film-type color for detecting volatile basic nitrogen gas characterized by spraying for 3 to 5 seconds through a 150 to 250um nozzle at a distance of 25 to 35 cm and heat treatment at 55 to 65 ° C for 1 to 3 minutes after application.
- a method of manufacturing a sensing device may be provided.
- the protective layer is spray-applied for 3 to 5 seconds at a distance of 25 to 35 cm from the surface of the color-sensing layer at a pressure of 35 to 45 psi, and heat treated at 55 to 65 ° C for 1 to 3 minutes after application.
- a method for manufacturing a film-type color sensing device for detecting volatile basic nitrogen gas can be provided.
- the film-type color sensing device for detecting volatile basic nitrogen gas and its manufacturing method according to an embodiment of the present invention have excellent flexibility, elasticity, and adhesion through a spin coating process or spray coating process, so that users can easily use it, It has excellent color change confirmation for volatile basic nitrogen gas, making it possible to easily detect volatile basic nitrogen in various fields.
- the structure of covering the color sensing part with a PDMS protective layer with gas permeability and hydrophobic properties allows volatile basic nitrogen to pass through and prevents reactive dyes such as BCG or PR from leaking, making it possible to stably apply it to the food field. there is.
- Figure 1 is a side view showing the structure of a film-type color sensing device according to an embodiment of the present invention.
- Figure 2 is a photograph showing the color change according to the pH change of the reactive dye mounted on the color sensing unit.
- Figure 3 is a diagram showing the process by which the reactive dye of the color sensing unit acquires a resonance structure when it comes into contact with a basic substance.
- Figure 4 is result data showing the change in UV-VIS absorbance as pH increases.
- Figure 5 is a reference diagram for explaining a method of manufacturing a film-type color sensing device according to an embodiment of the present invention.
- Figure 6 is data showing the results of measuring the thickness and surface uniformity of a film-type color sensing device according to an embodiment of the present invention.
- Figure 7 is a photograph showing an experiment on the elasticity and adhesion of a film-type color sensing device according to an embodiment of the present invention.
- Figure 8 is result data showing the change in absorbance according to ammonia gas exposure concentration.
- Figure 9 is a photograph showing an ammonia gas exposure experiment conducted after attaching a film-type color sensing device to a helmet according to an embodiment of the present invention.
- Figure 10 is a photograph showing a food spoilage test conducted after attaching a film-type color sensing device according to an embodiment of the present invention to a food storage container.
- Figure 11 is a diagram of an enzyme and microorganism experiment conducted using a film-type color sensing device for detecting volatile basic nitrogen gas and a manufacturing method thereof according to an embodiment of the present invention.
- Figure 12 shows result data for various microorganisms detected using a film-type color detection device for detecting volatile basic nitrogen gas and its manufacturing method according to an embodiment of the present invention.
- Figure 13 is a photograph and result data for confirming the reusability of a film-type color sensing device for detecting volatile basic nitrogen gas and its manufacturing method according to an embodiment of the present invention.
- Figure 14 is a side view showing the structure of a film-type color sensing device according to another embodiment of the present invention.
- Figure 1 is a side view showing the structure of a film-type color sensing device according to an embodiment of the present invention
- Figure 2 is a photograph showing the color change according to the pH change of the reactive dye mounted on the color sensing unit
- Figure 3 is a color It is a diagram showing the process by which a branch reactive dye acquires a resonance structure when in contact with a basic substance
- Figure 4 is the result data showing the change in UV-VIS absorbance as pH increases
- Figure 5 is an example of the present invention.
- Figure 6 is data showing the results of measuring the thickness and surface uniformity of a film-type color sensing device according to an embodiment of the present invention
- Figure 7 is This is a photograph showing an experiment on the elasticity and adhesion of a film-type color sensing device according to an embodiment of the present invention
- Figure 8 is the result data showing the change in absorbance according to the ammonia gas exposure concentration
- Figure 9 is an example of the present invention.
- FIG. 10 is a photograph showing an ammonia gas exposure experiment conducted after attaching a film-type color sensing device according to an embodiment to a helmet
- Figure 10 is a photo showing an ammonia gas exposure experiment conducted after attaching a film-type color sensing device according to an embodiment of the present invention to a food storage container. It is a photograph showing a food spoilage experiment
- Figure 11 is a diagram of an enzyme and microorganism experiment conducted using a film-type color detection device according to an embodiment of the present invention
- Figure 12 is a film according to an embodiment of the present invention.
- Figure 13 is a photograph and result data for confirming the reusability of the film-type color detection device according to an embodiment of the present invention
- Figure 14 is This is a side view showing the structure of a film-type color sensing device according to another embodiment of the present invention.
- a film-type color sensing device may include a color sensing unit 100, a first polymer protecting unit 200, and a second polymer protecting unit 300.
- the film-type color detection device is easy for users to use and has a large area at a low manufacturing cost. After manufacturing, it shows excellent flexibility and high specificity for basic gases (e.g., volatile basic nitrogen), allowing basic gases to be easily detected. It may refer to a film-type sensor.
- basic gases e.g., volatile basic nitrogen
- the film-type color sensing device has a first polymer protection portion 200 and a second polymer protection portion 300 disposed on both sides with the color sensing portion 100 in between, so it can be provided as a three-layer structure. You can.
- the color sensing unit 100 may contain a predetermined reactive dye so that a color change occurs in response to a basic gas.
- basic gas can be defined as trimethylamine (TMA), dimethylamine (DMA), ammonia gas, etc., which are released when rotting food or waste decays, and include volatile basic nitrogen containing a significant portion of nitrogen.
- Reactive dyes change color in response to basic gases containing volatile base nitrogen, allowing users to easily and conveniently detect ammonia gas or tell whether food is spoiled with the naked eye.
- the reactive dyes are commercially available pH indicator dyes, including bromocresol green (BCG), phenol red (PR), methyl orange (MO), and methyl red (MR), which have high color changes between pH 4 and 6 and pH 6 and 8. ), litmus, methyle purple (MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and any one of the universal indicators can be used.
- BCG bromocresol green
- PR phenol red
- MO methyl orange
- MR methyl red
- litmus methyle purple
- MP bromcresol purple
- bromthymol blue neutral red
- neutral red phenol red
- phenolphthalein phenolphthalein
- any one of the universal indicators can be used.
- FIG 2 is a photograph showing the color change according to the pH change of the reactive dye mounted on the color sensing unit 100.
- BCG Biscresol green
- PR phenol red
- the wavelength corresponding to the yellow color of the reactive dye of the color sensing unit 100 decreases, and the wavelength corresponding to the blue color (640 nm region, BCG) and the wavelength corresponding to the red color (570 nm region, PR) ) is showing an increase.
- the color sensing unit 100 containing a reactive dye with these characteristics can be manufactured in the form of a layer of a predetermined thickness through a spin coating method by mixing it with a solution of polydimethylsiloxane (PDMS), a polymer elastomer.
- PDMS polydimethylsiloxane
- a film-type color sensing device can be composed of a total of three functionalized layers.
- the first polymer protection part 200 and the second polymer protection part 300 are made of PDMS material with hydrophobicity and gas permeability to transmit basic gas and prevent reverse leakage of the reactive dye contained in the color sensing part 100. It can be.
- a film-type color sensing device according to an embodiment of the present invention can be manufactured through the following method.
- a PDMS solution can be made by mixing PDMS and PDMS curing agent at a mass ratio of 10:1.
- the polymer protective layer manufactured first is defined as the first polymer protective portion 200, and this first polymer protective portion 200 can be expressed as being disposed at the lowest layer in the drawing.
- the PDMS solution for manufacturing the first polymer protection part 200 was placed on the shelf 20 of the rotating means 10, and a spin coating method was performed to spread the PDMS solution to a predetermined thickness by rotating the rotating means 10 at a predetermined speed. Through subsequent heat curing, it can be finally produced in the form of a flexible film with a thickness of 15 to 25 um (optimum 20 um).
- the reactive dye BCG or PR
- a PDMS solution in which PDMS and PDMS curing agent were mixed at a mass ratio of 10:1. Afterwards, it can be placed on the top of the first polymer protection part 200 and the spin coating method as above can be performed.
- the color sensing part 100 in the form of a flexible film with a thickness of 55 to 65 um (optimum 60 um) can be created on the upper layer of the first polymer protection part 200 through heat curing. there is.
- the remaining second polymer protection unit 300 may be formed to be stacked on top of the color sensing unit 100.
- the second polymer protection part 300 is manufactured with the same composition and method as the first polymer protection part 200.
- PDMS and PDMS curing agent are mixed at a mass ratio of 10:1, spin coating is performed, and heat curing is performed to obtain a 15 It can be manufactured in the form of a flexible film with a thickness of ⁇ 25um.
- the thickness and surface uniformity of the film-type color sensing device manufactured by the above method were measured using a confocal microscope. Referring to FIG. 6, the color sensing portion 100 of approximately 60 nm and the first polymer protection of approximately 20 ⁇ m each were measured.
- the film-type color sensing device composed of the portion 200 and the second polymer protection portion 300 may be provided in the form of a flexible film with a total thickness of approximately 100 ⁇ m.
- the film-type color sensing device manufactured by this method has a three-layer structure in which the color sensing portion 100 is placed in the middle and the first polymer protecting portion 200 and the second polymer protecting portion 300 are disposed on both sides of the color sensing portion 100. It is provided in a (layer) structure, and the reason for arranging the first polymer protection part 200 and the second polymer protection part 300 on both sides of the color sensing part 100 is to protect the sensor through the gas permeability and hydrophobic properties of PDMS. This is to impose stability and gas selectivity.
- volatile base nitrogen gas can enter the interior, thereby causing color change.
- it can effectively prevent the reactive dye contained in the color sensing unit 100 from eluting out of the first polymer protection unit 200 and the second polymer protection unit 300, thereby reducing the risk of leakage of the reactive dye. It has the effect of providing stability.
- the film-type color sensing device has high reactivity to volatile basic nitrogen, which is a basic gas.
- the film-type color sensing device as described above is not only flexible, but also has excellent elasticity and adhesion as shown in FIG. 7, so it can be easily applied to various places (e.g., food packaging materials or containers, etc.) There is.
- a film-type color sensing device is exposed to ammonia gas, a type of volatile basic nitrogen, it can be confirmed that the color changes from yellow to blue, thereby improving the user's visual confirmation.
- the absorbance decreases at about 460 nm and increases in the 628 nm region, and the color sensing unit 100 is first exposed to the ammonia gas. It can be confirmed that the dehydrogenation reaction occurs efficiently inside the polymer protection unit 200 and the second polymer protection unit 300 and has resonance stability.
- the concentration of ammonia gas increases to about 50ppm or more, not only can a color change be detected with the naked eye, but it can also be seen that the increase in absorbance in the 628 nm region increases linearly according to the ammonia gas concentration.
- the film-type color sensing device has the advantage of being easily applicable to various industrial and food fields.
- the film-type color detection device according to this embodiment was attached to a safety helmet and an exposure experiment to ammonia gas was performed. As shown in FIG. 9, safety Exposure to ammonia gas can be easily confirmed by changing the color of the color sensing unit 100 attached to the helmet from yellow to blue.
- an agar medium containing urea shown in Figure 11 was prepared and enzyme and microorganism experiments were performed.
- ammonia is formed through a hydrolysis reaction between urea and urease contained in the medium, and this can be detected with the film-type color detection device according to this embodiment, confirming that the degree of ammonia emission increases depending on the concentration of urease. You can.
- urease-producing microorganisms can be detected for various microorganisms in agar medium containing urea as shown in the table in FIG. 12 using the film-type color detection device according to this embodiment.
- the color change of the color sensing unit 100 is related to the production of urease by microorganisms
- the color change was confirmed using an inhibitor that inhibits urease.
- the film-type color sensing device whose color changed by reacting with volatile base nitrogen gas was exposed to acetic acid gas or air to confirm reproducibility.
- a neutralization reaction with the adsorbed ammonia gas derivative was induced by exposure to fume generated from acetic acid (1N) liquid for 5 seconds, and it was confirmed that the color detection device returned to the color before exposure at 5 seconds of exposure.
- a film-type color sensing device may include a color sensing layer 400 and a protective layer 500.
- the film-type color sensing device according to another embodiment of the present invention is coated on a food resin material 30, such as kitchen wrap for food, by a spray method, and there is a difference in the manufacturing method.
- a food resin material 30 such as kitchen wrap for food
- only one protective layer 500 is required, resulting in a total two-layer structure, and has basically the same experimental results and effects as the mechanism of one embodiment of the present invention.
- the color-sensing layer 400 has basically the same structure as the color-sensing unit 100 described above and may refer to a layer applied by a spray method. Accordingly, the color-sensing layer 400 contains a predetermined reactive dye so that a color change occurs in response to a basic gas, and may be provided in the form of a layer with a predetermined thickness on the surface of the food resin material 30.
- the reactive dyes are commercially available pH indicator dyes, including bromocresol green (BCG), phenol red (PR), methyl orange (MO), methyl red (MR), litmus, and methyle purple ( Any one of MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and universal indicator can be used.
- BCG bromocresol green
- PR phenol red
- MO methyl orange
- MR methyl red
- litmus methyle purple
- methyle purple Any one of MP
- bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and universal indicator can be used.
- the color-sensing layer 400 is made by mixing a reactive dye in a PDMS solution, stirring it, diluting it using a hexane solution, applying it to the food resin material 30 using a spray method, and then heat-treating it to obtain a predetermined thickness. It may be provided in the form of a coating layer having a coating layer.
- the color-sensing layer 400 can be manufactured by the following method.
- the protective layer 500 has a similar structure to the first polymer protection part 200 or the second polymer protection part 300, and has a color sensing part 100 corresponding to the opposite side of the food resin material 30. It is laminated on one side and can be made of PDMS material with hydrophobicity and permeability to allow basic gas to pass through and to prevent leakage of reactive dye.
- the protective layer 500 is provided in the form of a coating layer surrounding the color-sensing layer 400 by applying a PDMS solution mixed with PDMS and PDMS curing agent on the surface of the color-sensing layer 400 through a spray method and then heat-treating it under predetermined conditions. It can be.
- the protective layer 500 is spray-applied with a PDMS solution at a pressure of 35-45 psi for 3-5 seconds at a distance of 25-35 cm from the surface of the color-sensing layer 400, and then applied at a pressure of 55-45 psi for 1-3 minutes. It can be prepared by heat treatment at 65°C.
- the film-type color sensing device sequentially laminates and coats the color sensing layer 400 and the protective layer 500 on a food resin material 30, such as kitchen wrap for food, through a spray method.
- a food resin material 30, such as kitchen wrap for food a food resin material 30, such as kitchen wrap for food
- the film-type color sensing device for detecting volatile basic nitrogen gas according to an embodiment of the present invention and its manufacturing method have been described as specific embodiments, but this is only an example and the present invention is not limited thereto, and the disclosure disclosed herein It should be interpreted as having the widest scope according to the basic idea.
- a person skilled in the art may combine and substitute the disclosed embodiments to implement embodiments not specified, but this also does not deviate from the scope of the present invention.
- a person skilled in the art can easily change or modify the embodiments disclosed based on the present specification, and it is clear that such changes or modifications also fall within the scope of the present invention.
- the present invention relates to a film-type color sensing device for detecting volatile basic nitrogen gas and a method of manufacturing the same, and can be used industrially.
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Abstract
The present invention relates to a film-type color-sensing device for detecting volatile basic nitrogen gas and a manufacturing method therefor. According to an embodiment, a film-type color-sensing device for detecting volatile basic nitrogen gas may be provided, the device comprising: a color-sensing part, which forms a layer of a preset thickness and comprises a predetermined reactive dye so as to produce a color change in response to a basic gas; a first polymer protection part, which is laminated on one side of the color-sensing part, with the color-sensing part in the middle, and is made of a hydrophobic and gas-permeable PDMS material, so as to allow the basic gas to pass there-through while preventing the reactive dye from leaking out; and a second polymer protection part, which is laminated on the other side of the color-sensing part, with the color-sensing part in the middle, and is made of a hydrophobic and gas-permeable PDMS material, so as to allow the basic gas to pass there-through while preventing the reactive dye from leaking out.
Description
본 발명은 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치 및 그 제조방법에 관한 것이다.The present invention relates to a film-type color sensing device for detecting volatile basic nitrogen gas and a method of manufacturing the same.
일반적으로, 암모니아는 '고압가스안전관리법' 및 '화학물질관리법'에서 가연성, 독성 유해화학 물질로 지정되어 있으나, 다양한 산업 분야에서 냉매로서의 성능이 우수하기 때문에 많이 사용되고 있는 실정이다.In general, ammonia is designated as a flammable, toxic and hazardous chemical in the 'High Pressure Gas Safety Management Act' and the 'Chemical Substances Control Act', but it is widely used in various industrial fields because of its excellent performance as a refrigerant.
특히 시설 노후화 등의 문제로 인하여 암모니아의 미세 누출이 발생될 수 있는데, 암모니아 누출 사고로 다수의 사상자가 발생한 경우도 심심치 않게 보고되고 있다.In particular, micro-leakage of ammonia may occur due to problems such as aging facilities, and cases of multiple casualties due to ammonia leakage accidents are frequently reported.
이에 The Occupational Safety and Health Administration(OSHA)에서는 8시간 노동에서 암모니아의 누출을 50ppm 이하로 제한하고 있는 바, 이 제한 농도 이상의 암모니아에 노출시 눈, 코, 인후, 기도 등에 작열감을 초래할 수 있다고 알려져 있다.Accordingly, the Occupational Safety and Health Administration (OSHA) limits the leakage of ammonia to less than 50ppm in an 8-hour workday. It is known that exposure to ammonia above this limit can cause a burning sensation in the eyes, nose, throat, and respiratory tract. .
한편, 식품 산업 분야에서 육류 및 어패류의 신선도가 감소함에 따라 증식한 미생물(부패 세균)의 효소 작용에 의해 단백질이 아미노산으로 분해되고, 아미노산은 다시 탈카르복실화에 의해 휘발성 아민류로 변화된다.Meanwhile, in the food industry, as the freshness of meat and fish and shellfish decreases, proteins are decomposed into amino acids by the enzymatic action of proliferating microorganisms (spoilage bacteria), and the amino acids are then changed into volatile amines through decarboxylation.
이와 같이 육류 및 어패류의 신선도가 감소하게 되는 과정에서 휘발성 암모니아 질소, 트리메틸아민(Trimethylamine), 다이메틸아민(Dimethylamine) 등(이하, "휘발성 염기질소(Total Volatile Basic Nitrogen; TVBN)"라 한다)이 생성되는 바, 이 휘발성 염기질소는 육류 및 어패류의 신선도를 알 수 있는 중요 지표로 사용될 수 있다.In the process of reducing the freshness of meat and fish and shellfish, volatile ammonia nitrogen, trimethylamine, dimethylamine, etc. (hereinafter referred to as “Total Volatile Basic Nitrogen (TVBN)”) are released. As it is produced, this volatile basic nitrogen can be used as an important indicator of the freshness of meat and fish and shellfish.
산업 현장에서 암모니아성 기체의 검출은 반도체식 가스 센서를 이용하거나 광센서 기반 센서 시스템을 공장에 설치하여 사용하는 것이 일반적이지만, 이러한 센서의 경우 높은 가격 등으로 인하여 소규모 현장에서는 사용이 어려운 문제가 있다.It is common to detect ammonia gas in industrial sites by using semiconductor gas sensors or installing optical sensor-based sensor systems in factories, but these sensors are difficult to use in small-scale sites due to their high prices. .
또한 식품 산업 분야에서 식품 부패를 검출하기 위해 반도체식 가스 센서와 광센서 기반의 시스템을 육류 및 어패류 포장 내부에 동봉하는 것은 현실적으로 불가능한 문제가 있다.Additionally, in the food industry, it is realistically impossible to enclose a semiconductor gas sensor and optical sensor-based system inside meat and seafood packaging to detect food spoilage.
식품 포장에 동봉되기 위한 센서의 경우 유연성 및 접착성 그리고 육류 및 어패류에서 나오는 수분 등의 방해 물질에 영향을 받지 않으면서 휘발성 아민에만 선택적으로 반응할 수 있고, 사용자가 음식의 신선도를 간편하게 알 수 있어야 한다.In the case of a sensor to be included in food packaging, it must have flexibility, adhesiveness, and be able to respond selectively to volatile amines without being affected by interfering substances such as moisture from meat and fish and shellfish, and allow users to easily know the freshness of food. do.
또한 높은 재현성 및 응용을 위해 센서 제작 공정이 비교적 단순하고, 대면적화가 가능해야 하며, 산업 현장에서 현장 노동자 및 식품 구매자들이 손쉽게 사용 및 폐기가 가능해야 하므로, 이러한 제반 요건을 충족할 수 있는 휘발성 염기 질소 가스 검출을 위한 센서의 개발이 요구되고 있다.In addition, for high reproducibility and application, the sensor manufacturing process must be relatively simple, large-scale, and easy to use and dispose of by workers and food purchasers in industrial sites, so a volatile base that can meet these requirements is needed. The development of sensors for nitrogen gas detection is required.
본 발명의 일 실시예에 따른 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치 및 그 제조방법은 상기와 같은 문제를 해결하기 위해 제안된 것으로서, 사용자가 간편하게 사용하면서 저가로 대면적화가 가능하고 유연성을 갖추며 휘발성 염기질소 및 암모니아 기체에 높은 특이성을 갖도록 하는데 그 목적이 있다.A film-type color sensing device for detecting volatile basic nitrogen gas and a manufacturing method thereof according to an embodiment of the present invention were proposed to solve the above problems, and are easy for users to use, can be expanded to a large area at low cost, and are flexible. The purpose is to have high specificity for volatile basic nitrogen and ammonia gas.
일 실시예에 따르면, 염기성 가스에 반응하여 색 변화가 발생하도록 소정의 반응 염료를 포함하며, 소정 두께의 층(layer) 형상으로 제공되는 색감지부; 상기 색감지부를 사이에 두고 그 일측면에 적층되며, 상기 염기성 가스는 투과시키고 상기 반응 염료의 누출은 방지하기 위해 소수성 및 기체 투과성을 갖는 PDMS 소재로 제공되는 제1고분자보호부; 및 상기 색감지부를 사이에 두고 그 타측면에 적층되며, 상기 염기성 가스는 투과시키고 상기 반응 염료의 누출은 방지하기 위해 소수성 및 기체 투과성을 갖는 PDMS 소재로 제공되는 제2고분자보호부;를 포함하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.According to one embodiment, a color sensing unit includes a predetermined reactive dye so that a color change occurs in response to a basic gas, and is provided in the form of a layer with a predetermined thickness; A first polymer protection part laminated on one side of the color sensing part with the color sensing part in between, and made of PDMS material having hydrophobicity and gas permeability to transmit the basic gas and prevent leakage of the reactive dye; And a second polymer protection part laminated on the other side of the color sensing part with the color sensing part in between, and made of PDMS material having hydrophobicity and gas permeability to transmit the basic gas and prevent leakage of the reactive dye. , a film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
또한, 상기 염기성 가스는 휘발성 염기 질소인 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.Additionally, a film-type color sensing device for detecting volatile basic nitrogen gas may be provided, wherein the basic gas is volatile basic nitrogen.
또한, 상기 반응 염료는 pH 지시약 상용 염료로서, pH 4~8 사이에서 색변화를 갖는 Bromocresol green(BCG), phenol red(PR), methyl orange(MO), methyl red(MR), litmus, methyle purple(MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein 및 universal indicator 중 어느 하나가 사용된 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.In addition, the reactive dyes are commercial pH indicator dyes, such as bromocresol green (BCG), phenol red (PR), methyl orange (MO), methyl red (MR), litmus, and methyle purple, which change color between pH 4 and 8. A film-type color detection device for detecting volatile basic nitrogen gas may be provided, characterized in that any one of (MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and universal indicator is used.
또한, 상기 색감지부는 PDMS와 PDMS 경화제가 10:1의 질량비로 혼합된 PDMS용액에 상기 반응 염료를 혼합하고 스핀코팅 공법을 수행한 후 열 경화를 통해 55~65um의 두께를 갖는 유연한 필름 형태로 제공되는 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.In addition, the color sensing unit mixes the reactive dye with a PDMS solution in which PDMS and PDMS curing agent are mixed at a mass ratio of 10:1, performs spin coating, and then thermally cures it to form a flexible film with a thickness of 55 to 65 um. A film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
또한, 상기 제1고분자보호부 및 상기 제2고분자보호부는 PDMS와 PDMS 경화제를 10:1의 질량비로 혼합하여 스핀코팅 공법을 수행하고 열경화를 통해 15~25um의 두께를 갖는 유연한 필름 형태로 제공되는 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.In addition, the first polymer protection part and the second polymer protection part are provided in the form of a flexible film with a thickness of 15 to 25 um through spin coating by mixing PDMS and PDMS curing agent at a mass ratio of 10:1 and heat curing. A film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
일 실시예에 따르면, PDMS와 PDMS경화제를 10:1의 질량비로 혼합하여 PDMS용액을 만드는 단계; 상기 PDMS용액을 회전수단에 올려 놓고 소정 속도로 회전시켜 소정 두께로 펴는 스핀코팅 공법을 수행하고, 열 경화를 통해 유연한 필름 형태의 제1고분자보호부를 형성하는 단계; PDMS와 PDMS경화제가 10:1의 질량비로 혼합된 PDMS용액에 반응 염료를 혼합한 후 이를 상기 제1고분자보호부의 상부에 올려놓고 스핀코팅 공법을 수행하고 열 경화를 통해 상기 제1고분자보호부의 상부에 유연한 필름 형태의 색감지부를 형성하는 단계; 및 상기 PDMS용액을 상기 색감지부의 상부에 올려 놓고 스핀코팅 공법을 수행한 후 열 경화를 통해 상기 색감지부의 상부에 유연한 필름 형태의 제2고분자보호부를 형성하는 단계;를 포함하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법이 제공될 수 있다.According to one embodiment, mixing PDMS and PDMS curing agent at a mass ratio of 10:1 to prepare a PDMS solution; Performing a spin coating method of placing the PDMS solution on a rotating means and rotating it at a predetermined speed to spread it to a predetermined thickness, and forming a first polymer protection part in the form of a flexible film through heat curing; After mixing the reactive dye with the PDMS solution in which PDMS and PDMS curing agent are mixed at a mass ratio of 10:1, it is placed on the top of the first polymer protective part, a spin coating process is performed, and the upper part of the first polymer protective part is formed through heat curing. forming a color sensing unit in the form of a flexible film; And placing the PDMS solution on top of the color-sensing part, performing a spin coating method, and then forming a second polymer protection part in the form of a flexible film on the upper part of the color-sensing part through heat curing. Volatile basic nitrogen comprising a. A method of manufacturing a film-type color sensing device for gas detection can be provided.
또한, 상기 제1고분자보호부 및 상기 제2고분자보호부는 15~25um의 두께를 가지고, 상기 색감지부는 55~65um의 두께를 갖도록 제조되는 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법이 제공될 수 있다.In addition, the first polymer protection part and the second polymer protection part are manufactured to have a thickness of 15 to 25 um, and the color sensing part is manufactured to have a thickness of 55 to 65 um. A method of manufacturing a color sensing device may be provided.
일 실시예에 따르면, 염기성 가스에 반응하여 색 변화가 발생하도록 소정의 반응 염료를 포함하며, 식품용 수지재의 표면 상에 소정 두께의 층(layer) 형상으로 제공되는 색감지층; 및 상기 식품용 수지재의 반대측에 해당하는 상기 색감지부의 일측면에 적층되며, 상기 염기성 가스는 투과시키고 상기 반응 염료의 누출은 방지하기 위해 소수성 및 기체 투과성을 갖는 PDMS 소재로 제공되는 보호층;을 포함하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.According to one embodiment, a color-sensing layer includes a predetermined reactive dye so that a color change occurs in response to a basic gas, and is provided in the form of a layer of a predetermined thickness on the surface of a food resin material; and a protective layer laminated on one side of the color sensing unit corresponding to the opposite side of the food resin material and made of PDMS material having hydrophobicity and gas permeability to transmit the basic gas and prevent leakage of the reactive dye. A film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
또한, 상기 염기성 가스는 휘발성 염기 질소인 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.Additionally, a film-type color sensing device for detecting volatile basic nitrogen gas may be provided, wherein the basic gas is volatile basic nitrogen.
또한, 상기 반응 염료는 pH 지시약 상용 염료로서, pH 4~8 사이에서 색변화를 갖는 Bromocresol green(BCG), phenol red(PR), methyl orange(MO), methyl red(MR), litmus, methyle purple(MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein 및 universal indicator 중 어느 하나가 사용된 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.In addition, the reactive dyes are commercial pH indicator dyes, such as bromocresol green (BCG), phenol red (PR), methyl orange (MO), methyl red (MR), litmus, and methyle purple, which change color between pH 4 and 8. A film-type color detection device for detecting volatile basic nitrogen gas may be provided, characterized in that any one of (MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and universal indicator is used.
또한, 상기 색감지층은 PDMS용액에 상기 반응 염료를 혼합하여 교반한 후 hexane 용액을 사용하여 희석하고, 이를 스프레이 공법을 수행하여 상기 식품용 수지재에 도포한 후 소정 조건에서의 열처리하는 과정을 통하여 코팅층 형태로 제공되는 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.In addition, the color-sensing layer is created by mixing and stirring the reactive dye in the PDMS solution, diluting it with a hexane solution, applying it to the food resin material by spraying it, and then heat-treating it under predetermined conditions. A film-type color sensing device for detecting volatile basic nitrogen gas may be provided, characterized in that it is provided in the form of a coating layer.
또한, 상기 색감지층은, 상기 PDMS용액에 상기 반응염료를 혼합하여 22~26시간 100~300rpm에서 교반하고, hexane용액을 사용하여 희석하고 나면, 35~45psi의 압력으로 상기 식품용 수지재의 표면에서 25~35cm의 거리를 두고 150~250um 노즐을 통해 3~5초간 스프레이 도포하며, 도포후 1~3분간 55~65 ℃에서 열처리하는 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.In addition, the color sensing layer is mixed with the reactive dye in the PDMS solution, stirred at 100 to 300 rpm for 22 to 26 hours, and diluted with a hexane solution, and then applied to the surface of the food resin material at a pressure of 35 to 45 psi. Film-type color detection for detecting volatile basic nitrogen gas, characterized by spraying for 3 to 5 seconds through a 150 to 250um nozzle at a distance of 25 to 35 cm and heat treatment at 55 to 65 ° C for 1 to 3 minutes after application. A device may be provided.
또한, 상기 보호층은 PDMS와 PDMS 경화제가 혼합된 PDMS용액을 스프레이 공법을 통하여 상기 색감지층의 표면상에 도포한 후 소정 조건에서 열처리하는 과정을 통하여 상기 색감지층을 감싸는 코팅층 형태로 제공되는 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.In addition, the protective layer is provided in the form of a coating layer surrounding the color-sensing layer by applying a PDMS solution mixed with PDMS and PDMS curing agent on the surface of the color-sensing layer through a spray method and then heat-treating it under predetermined conditions. A film-type color sensing device for detecting volatile basic nitrogen gas can be provided.
또한, 상기 보호층은 상기 PDMS용액을 35~45psi의 압력으로 상기 색감지층의 표면에서 25~35cm의 거리를 두고 3~5초간 스프레이 도포하고, 도포 후 1~3분간 55~65 ℃에서 열처리하는 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치가 제공될 수 있다.In addition, the protective layer is spray-applied for 3 to 5 seconds at a distance of 25 to 35 cm from the surface of the color-sensing layer at a pressure of 35 to 45 psi, and heat treated at 55 to 65 ° C for 1 to 3 minutes after application. A film-type color sensing device for detecting volatile basic nitrogen gas may be provided.
일 실시예에 따르면, PDMS용액에 반응 염료를 혼합하여 교반한 후 hexane용액을 사용하여 희석한 다음 이를 소정 압력으로 식품용 수지재의 표면 상에 스프레이 도포하는 단계; 스프레이 도포 후 소정 조건에서 열처리하여 코팅층 형태의 색감지층을 형성하는 단계; 상기 색감지층이 형성된 후 PDMS용액을 상기 색감지층의 표면상에 도포하는 단계; 및 상기 PDMS용액을 도포한 후 소정 조건에서 열처리하여 상기 색감지층을 감싸는 코팅층 형태의 보호층을 형성하는 단계;를 포함하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법이 제공될 수 있다.According to one embodiment, mixing and stirring a reactive dye in a PDMS solution, diluting it with a hexane solution, and spraying it on the surface of a food resin material at a predetermined pressure; Forming a color-sensitive layer in the form of a coating layer by heat-treating it under predetermined conditions after spray application; After the color-sensing layer is formed, applying a PDMS solution onto the surface of the color-sensing layer; and applying the PDMS solution and then heat-treating it under predetermined conditions to form a protective layer in the form of a coating layer surrounding the color-sensing layer. A method of manufacturing a film-type color sensing device for detecting volatile basic nitrogen gas will be provided, including You can.
또한, 상기 색감지층은, 상기 PDMS용액에 상기 반응염료를 혼합하여 22~26시간, 100~300rpm에서 교반하고, hexane용액을 사용하여 희석하고 나면, 35~45psi의 압력으로 상기 식품용 수지재의 표면에서 25~35cm의 거리를 두고 150~250um 노즐을 통해 3~5초간 스프레이 도포하며, 도포후 1~3분간 55~65 ℃에서 열처리하는 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법이 제공될 수 있다.In addition, the color sensing layer is mixed with the reactive dye in the PDMS solution, stirred at 100 to 300 rpm for 22 to 26 hours, and diluted with a hexane solution, and then applied to the surface of the food resin material at a pressure of 35 to 45 psi. Film-type color for detecting volatile basic nitrogen gas, characterized by spraying for 3 to 5 seconds through a 150 to 250um nozzle at a distance of 25 to 35 cm and heat treatment at 55 to 65 ° C for 1 to 3 minutes after application. A method of manufacturing a sensing device may be provided.
또한, 상기 보호층은 상기 PDMS용액을 35~45psi의 압력으로 상기 색감지층의 표면에서 25~35cm의 거리를 두고 3~5초간 스프레이 도포하고, 도포 후 1~3분간 55~65 ℃에서 열처리하는 것을 특징으로 하는, 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법이 제공될 수 있다.In addition, the protective layer is spray-applied for 3 to 5 seconds at a distance of 25 to 35 cm from the surface of the color-sensing layer at a pressure of 35 to 45 psi, and heat treated at 55 to 65 ° C for 1 to 3 minutes after application. A method for manufacturing a film-type color sensing device for detecting volatile basic nitrogen gas can be provided.
본 발명의 일 실시예에 따른 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치 및 그 제조방법은 스핀코팅 공정 또는 스프레이코팅 공정을 통해 유연성, 신축성, 부착성이 우수하여 사용자가 간편하게 사용할 수 있고, 휘발성 염기질소 가스에 대한 색변화 확인성이 우수하여 다양한 분야에서 휘발성 염기질소를 용이하게 검출할 수 있는 효과가 있다.The film-type color sensing device for detecting volatile basic nitrogen gas and its manufacturing method according to an embodiment of the present invention have excellent flexibility, elasticity, and adhesion through a spin coating process or spray coating process, so that users can easily use it, It has excellent color change confirmation for volatile basic nitrogen gas, making it possible to easily detect volatile basic nitrogen in various fields.
또한, 색감지부를 기체 투과성과 소수성 특성을 갖는 PDMS 보호층으로 감싸는 구조에 의하여 휘발성 염기질소는 통과시키고 BCG 또는 PR 등의 반응 염료가 누출되는 것을 방지함으로써 식품 분야에도 안정적으로 적용할 수 있는 효과가 있다.In addition, the structure of covering the color sensing part with a PDMS protective layer with gas permeability and hydrophobic properties allows volatile basic nitrogen to pass through and prevents reactive dyes such as BCG or PR from leaking, making it possible to stably apply it to the food field. there is.
또한, 3단계의 스핀코팅 공정 또는 2단계의 스프레이코팅 공정을 통한 고분자 용액을 사용하여 대면적화할 수 있고 높은 공정성을 확보할 수 있는 장점이 있다.In addition, it has the advantage of being able to expand to a large area and ensure high processability by using a polymer solution through a three-step spin coating process or a two-step spray coating process.
또한, 휘발성 염기질소 가스에 노출될 수 있는 다양한 산업 분야에 적용이 가능하며, 식품 분야에 적용하여 육류 및 어류의 부패를 빠르게 인지할 수 있고, urease-효소 생성 미생물 분야에서도 암모니아 기체의 검출에 사용될 수 있는 바, 다양한 분야에 폭 넓게 응용이 가능한 장점이 있다.In addition, it can be applied to various industrial fields that can be exposed to volatile basic nitrogen gas, and can be applied to the food field to quickly recognize spoilage of meat and fish, and can also be used to detect ammonia gas in the field of urease-enzyme producing microorganisms. It has the advantage of being widely applicable to various fields.
도 1은 본 발명의 일 실시예에 따른 필름형 색 감지장치의 구조를 도시한 측면도이다.Figure 1 is a side view showing the structure of a film-type color sensing device according to an embodiment of the present invention.
도 2는 색감지부에 탑재되는 반응 염료의 pH 변화에 따른 색 변화를 나타낸 사진이다.Figure 2 is a photograph showing the color change according to the pH change of the reactive dye mounted on the color sensing unit.
도 3은 색감지부의 반응 염료가 염기성 물질과 접촉시 공명 구조를 갖게 되는 과정을 도시한 도면이다.Figure 3 is a diagram showing the process by which the reactive dye of the color sensing unit acquires a resonance structure when it comes into contact with a basic substance.
도 4는 pH 증가에 따른 UV-VIS 흡광도 변화를 도시한 결과 데이터이다.Figure 4 is result data showing the change in UV-VIS absorbance as pH increases.
도 5는 본 발명의 일 실시예에 따른 필름형 색 감지장치의 제조 방법을 설명하기 위한 참고도이다.Figure 5 is a reference diagram for explaining a method of manufacturing a film-type color sensing device according to an embodiment of the present invention.
도 6은 본 발명의 일 실시예에 따른 필름형 색 감지장치의 두께 및 표면 균일성을 측정한 결과 데이터이다.Figure 6 is data showing the results of measuring the thickness and surface uniformity of a film-type color sensing device according to an embodiment of the present invention.
도 7은 본 발명의 일 실시예에 따른 필름형 색 감지장치의 신축성, 부착성에 대한 실험을 보여주는 사진이다.Figure 7 is a photograph showing an experiment on the elasticity and adhesion of a film-type color sensing device according to an embodiment of the present invention.
도 8은 암모니아 가스 노출 농도에 따른 흡광도 변화를 도시한 결과 데이터이다.Figure 8 is result data showing the change in absorbance according to ammonia gas exposure concentration.
도 9는 본 발명의 일 실시예에 따른 필름형 색 감지장치를 헬멧에 부착 후 진행한 암모니아 기체 노출 실험을 보여주는 사진이다.Figure 9 is a photograph showing an ammonia gas exposure experiment conducted after attaching a film-type color sensing device to a helmet according to an embodiment of the present invention.
도 10은 본 발명의 일 실시예에 따른 필름형 색 감지장치를 식품 보관 용기에 부착후 진행한 식품 부패 실험을 보여주는 사진이다.Figure 10 is a photograph showing a food spoilage test conducted after attaching a film-type color sensing device according to an embodiment of the present invention to a food storage container.
도 11은 본 발명의 일 실시예에 따른 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치 및 그 제조방법을 이용하여 진행한 효소 및 미생물 실험에 대한 도면이다.Figure 11 is a diagram of an enzyme and microorganism experiment conducted using a film-type color sensing device for detecting volatile basic nitrogen gas and a manufacturing method thereof according to an embodiment of the present invention.
도 12는 본 발명의 일 실시예에 따른 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치 및 그 제조방법을 이용하여 검출한 다양한 미생물을 대상으로 한 결과 데이터이다.Figure 12 shows result data for various microorganisms detected using a film-type color detection device for detecting volatile basic nitrogen gas and its manufacturing method according to an embodiment of the present invention.
도 13은 본 발명의 일 실시예에 따른 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치 및 그 제조방법의 재사용성 확인을 위한 사진 및 결과 데이터이다.Figure 13 is a photograph and result data for confirming the reusability of a film-type color sensing device for detecting volatile basic nitrogen gas and its manufacturing method according to an embodiment of the present invention.
도 14는 본 발명의 다른 실시예에 따른 필름형 색 감지장치의 구조를 도시한 측면도이다.Figure 14 is a side view showing the structure of a film-type color sensing device according to another embodiment of the present invention.
이하에서는 본 발명의 구체적인 실시예들에 대하여 도면을 참조하여 상세히 설명한다. 아울러 본 발명을 설명함에 있어서, 관련된 공지 구성 또는 기능에 대한 구체적인 설명이 본 발명의 요지를 흐릴 수 있다고 판단되는 경우에는 그 상세한 설명을 생략한다.Hereinafter, specific embodiments of the present invention will be described in detail with reference to the drawings. In addition, when describing the present invention, if it is determined that a detailed description of a related known configuration or function may obscure the gist of the present invention, the detailed description will be omitted.
이하의 설명은 특허 청구 가능한 본 발명의 여러 측면 중 하나이며, 하기의 설명은 본 발명에 대한 상세한 기술의 일부를 이룰 수 있다. 본 발명은 다양한 변경을 가할 수 있고 여러 가지 실시예들을 포함할 수 있는 바, 특정 실시예들을 도면에 예시하고 상세한 설명을 통해 설명할 수 있다.The following description is one of several aspects of the invention that may be claimed for patent, and may form part of a detailed description of the invention. The present invention can make various changes and include various embodiments, and specific embodiments may be illustrated in the drawings and described in detail.
그러나 이는 본 발명의 특정한 실시 형태에 대해 한정하려는 것은 아니며, 본 발명의 사상 및 기술 범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다.However, this is not intended to limit the present invention to specific embodiments, and should be understood to include all changes, equivalents, and substitutes included in the spirit and technical scope of the present invention.
제1, 제2 등과 같이 서수를 포함하는 용어는 다양한 구성요소들을 설명하는데 사용될 수 있지만, 해당 구성요소들은 이와 같은 용어들에 의해 한정되지는 않는다. 이 용어들은 하나의 구성요소들을 다른 구성요소로부터 구별하는 목적으로만 사용된다.Terms including ordinal numbers, such as first, second, etc., may be used to describe various components, but the components are not limited by these terms. These terms are used only to distinguish one component from another.
본 출원에서 사용한 용어는 단지 특정한 실시예를 설명하기 위해 사용된 것으로, 본 발명을 한정하려는 의도가 아니다. 단수의 표현은 문맥상 명백하게 다르게 뜻하지 않는 한, 복수의 표현을 포함한다.The terms used in this application are only used to describe specific embodiments and are not intended to limit the invention. Singular expressions include plural expressions unless the context clearly dictates otherwise.
이하, 첨부된 도면을 참조하여 본 발명의 일 실시예에 대하여 상세하게 설명한다.Hereinafter, an embodiment of the present invention will be described in detail with reference to the attached drawings.
도 1은 본 발명의 일 실시예에 따른 필름형 색 감지장치의 구조를 도시한 측면도이고, 도 2는 색감지부에 탑재되는 반응 염료의 pH 변화에 따른 색 변화를 나타낸 사진이며, 도 3은 색감지부의 반응 염료가 염기성 물질과 접촉시 공명 구조를 갖게 되는 과정을 도시한 도면이고, 도 4는 pH 증가에 따른 UV-VIS 흡광도 변화를 도시한 결과 데이터이며, 도 5는 본 발명의 일 실시예에 따른 필름형 색 감지장치의 제조 방법을 설명하기 위한 참고도이고, 도 6은 본 발명의 일 실시예에 따른 필름형 색 감지장치의 두께 및 표면 균일성을 측정한 결과 데이터이며, 도 7은 본 발명의 일 실시예에 따른 필름형 색 감지장치의 신축성, 부착성에 대한 실험을 보여주는 사진이고, 도 8은 암모니아 가스 노출 농도에 따른 흡광도 변화를 도시한 결과 데이터이며, 도 9는 본 발명의 일 실시예에 따른 필름형 색 감지장치를 헬멧에 부착 후 진행한 암모니아 기체 노출 실험을 보여주는 사진이고, 도 10은 본 발명의 일 실시예에 따른 필름형 색 감지장치를 식품 보관 용기에 부착후 진행한 식품 부패 실험을 보여주는 사진이며, 도 11은 본 발명의 일 실시예에 따른 필름형 색 감지장치를 이용하여 진행한 효소 및 미생물 실험에 대한 도면이고, 도 12는 본 발명의 일 실시예에 따른 필름형 색 감지장치를 이용하여 검출한 다양한 미생물을 대상으로 한 결과 데이터이며, 도 13은 본 발명의 일 실시예에 따른 필름형 색 감지장치의 재사용성 확인을 위한 사진 및 결과 데이터이고, 도 14는 본 발명의 다른 실시예에 따른 필름형 색 감지장치의 구조를 도시한 측면도이다.Figure 1 is a side view showing the structure of a film-type color sensing device according to an embodiment of the present invention, Figure 2 is a photograph showing the color change according to the pH change of the reactive dye mounted on the color sensing unit, and Figure 3 is a color It is a diagram showing the process by which a branch reactive dye acquires a resonance structure when in contact with a basic substance, Figure 4 is the result data showing the change in UV-VIS absorbance as pH increases, and Figure 5 is an example of the present invention. It is a reference diagram for explaining the manufacturing method of a film-type color sensing device according to , Figure 6 is data showing the results of measuring the thickness and surface uniformity of a film-type color sensing device according to an embodiment of the present invention, and Figure 7 is This is a photograph showing an experiment on the elasticity and adhesion of a film-type color sensing device according to an embodiment of the present invention, Figure 8 is the result data showing the change in absorbance according to the ammonia gas exposure concentration, and Figure 9 is an example of the present invention. This is a photograph showing an ammonia gas exposure experiment conducted after attaching a film-type color sensing device according to an embodiment to a helmet, and Figure 10 is a photo showing an ammonia gas exposure experiment conducted after attaching a film-type color sensing device according to an embodiment of the present invention to a food storage container. It is a photograph showing a food spoilage experiment, and Figure 11 is a diagram of an enzyme and microorganism experiment conducted using a film-type color detection device according to an embodiment of the present invention, and Figure 12 is a film according to an embodiment of the present invention. This is the result data targeting various microorganisms detected using a color detection device, Figure 13 is a photograph and result data for confirming the reusability of the film-type color detection device according to an embodiment of the present invention, and Figure 14 is This is a side view showing the structure of a film-type color sensing device according to another embodiment of the present invention.
도 1을 참조하면, 본 발명의 일 실시예에 따른 필름형 색 감지장치는 색감지부(100), 제1고분자보호부(200) 및 제2고분자보호부(300)를 포함할 수 있다.Referring to FIG. 1, a film-type color sensing device according to an embodiment of the present invention may include a color sensing unit 100, a first polymer protecting unit 200, and a second polymer protecting unit 300.
필름형 색 감지장치는 사용자가 간편하게 사용하면서 저렴한 제조 비용으로 대면적화가 가능하고, 제조 후 탁월한 유연성 및 염기성 가스(예컨대, 휘발성 염기 질소)에 높은 특이성을 보여 염기성 가스를 용이하게 검출할 수 있도록 하는 필름형 센서를 의미할 수 있다.The film-type color detection device is easy for users to use and has a large area at a low manufacturing cost. After manufacturing, it shows excellent flexibility and high specificity for basic gases (e.g., volatile basic nitrogen), allowing basic gases to be easily detected. It may refer to a film-type sensor.
필름형 색 감지장치는 색감지부(100)를 사이에 두고 그 양 측면에 제1고분자보호부(200) 및 제2고분자보호부(300)가 배치되므로, 총 3개의 층을 이루는 구조로 제공될 수 있다.The film-type color sensing device has a first polymer protection portion 200 and a second polymer protection portion 300 disposed on both sides with the color sensing portion 100 in between, so it can be provided as a three-layer structure. You can.
색감지부(100)는 염기성 가스에 반응하여 색 변화가 발생하도록 소정의 반응 염료를 포함할 수 있다. 여기서, 염기성 가스는 부패 식품 또는 폐기물 등이 부패할 때 나오는 트리메틸아민(TMA), 디메틸아민(DMA), 암모니아 가스 등으로 상당 부분 질소가 포함된 휘발성 염기 질소를 포함하는 개념으로 정의될 수 있다. The color sensing unit 100 may contain a predetermined reactive dye so that a color change occurs in response to a basic gas. Here, basic gas can be defined as trimethylamine (TMA), dimethylamine (DMA), ammonia gas, etc., which are released when rotting food or waste decays, and include volatile basic nitrogen containing a significant portion of nitrogen.
반응 염료는 이러한 휘발성 염기 질소를 포함하는 염기성 가스에 반응하여 색이 변화함으로써 사용자는 육안으로 암모니아 가스의 검출 또는 식품 등의 부패 여부를 쉽고 간편하게 알 수 있도록 해 준다.Reactive dyes change color in response to basic gases containing volatile base nitrogen, allowing users to easily and conveniently detect ammonia gas or tell whether food is spoiled with the naked eye.
구체적으로, 반응 염료는 pH 지시약 상용 염료로서, pH 4~6 및 pH 6~8 사이에서 높은 색변화를 갖는 Bromocresol green(BCG), phenol red(PR), methyl orange(MO), methyl red(MR), litmus, methyle purple(MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein 및 universal indicator 중 어느 하나가 사용될 수 있다.Specifically, the reactive dyes are commercially available pH indicator dyes, including bromocresol green (BCG), phenol red (PR), methyl orange (MO), and methyl red (MR), which have high color changes between pH 4 and 6 and pH 6 and 8. ), litmus, methyle purple (MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and any one of the universal indicators can be used.
도 2는 색감지부(100)에 탑재되는 반응 염료의 pH변화에 따른 색 변화를 나타낸 사진으로, 반응 염료에 사용되는 BCG(Bromocresol green) 또는 PR(phenol red)의 경우 염기성 물질과 접촉시 분명한 색변화를 보이게 된다. 도 2를 참조하면 BCG의 경우 pH가 증가할수록 노란색 계열에서 점차 파란색 계열로 색변화가 일어나는 것을 확인할 수 있으며, PR의 경우 pH가 증가할수록 노란색 계열에서 점차 빨간색 계열로 색변화가 일어나는 것을 확인할 수 있다.Figure 2 is a photograph showing the color change according to the pH change of the reactive dye mounted on the color sensing unit 100. In the case of BCG (Bromocresol green) or PR (phenol red) used in the reactive dye, the color is clear upon contact with a basic substance. You will see change. Referring to Figure 2, in the case of BCG, it can be seen that as the pH increases, the color changes from yellow to blue, and in the case of PR, as pH increases, the color changes from yellow to red. .
또한, 반응 염료의 BCG 또는 PR의 경우 염기성 물질에 노출되었을 때 도 3과 같은 탈수소화 반응으로 인하여 공명구조를 가지게 되고, 이러한 공명 구조의 안정화로 인해 UV-VIS 흡광도에서 red shift가 관찰될 수 있다.In addition, in the case of BCG or PR of reactive dyes, when exposed to basic substances, they have a resonance structure due to a dehydrogenation reaction as shown in Figure 3, and a red shift can be observed in UV-VIS absorbance due to stabilization of this resonance structure. .
도 4를 참조하면, pH가 증가함에 따라 색감지부(100)의 반응 염료의 노란색에 해당하는 파장이 줄어들고, 파란색에 해당하는 파장(640nm 영역, BCG) 및 빨간색에 해당하는 파장(570nm 영역, PR)이 증가하는 결과를 보이고 있다.Referring to FIG. 4, as the pH increases, the wavelength corresponding to the yellow color of the reactive dye of the color sensing unit 100 decreases, and the wavelength corresponding to the blue color (640 nm region, BCG) and the wavelength corresponding to the red color (570 nm region, PR) ) is showing an increase.
이러한 특성을 갖는 반응 염료를 포함하는 색감지부(100)는 고분자 엘라스토머(polymer elastomer)인 Polydimethylsiloxane(PDMS) 용액에 혼합하여 스핀코팅 공법을 통해 소정 두께의 층(layer) 형상으로 제조될 수 있다.The color sensing unit 100 containing a reactive dye with these characteristics can be manufactured in the form of a layer of a predetermined thickness through a spin coating method by mixing it with a solution of polydimethylsiloxane (PDMS), a polymer elastomer.
한편, 상기 색감지부(100)를 사이에 두고 그 일측면과 그 타측면에는 각각 제1고분자보호부(200) 및 제2고분자보호부(300)가 적층되는 바, 이에 따라 본 실시예에 따른 필름형 색 감지장치는 총 3층의 기능화 레이어로 구성될 수 있다.Meanwhile, a first polymer protection unit 200 and a second polymer protection unit 300 are stacked on one side and the other side with the color sensing unit 100 in between, respectively, according to the present embodiment. A film-type color sensing device can be composed of a total of three functionalized layers.
제1고분자보호부(200) 및 제2고분자보호부(300)는 염기성 가스는 투과시키고 색감지부(100)에 포함된 반응 염료의 역 누출은 방지하기 위해 소수성 및 기체 투과성을 갖는 PDMS 소재로 제공될 수 있다.The first polymer protection part 200 and the second polymer protection part 300 are made of PDMS material with hydrophobicity and gas permeability to transmit basic gas and prevent reverse leakage of the reactive dye contained in the color sensing part 100. It can be.
도 5를 참조하면, 본 발명의 일 실시예에 따른 필름형 색 감지장치는 아래와 같은 방법을 통해 제조될 수 있다.Referring to FIG. 5, a film-type color sensing device according to an embodiment of the present invention can be manufactured through the following method.
먼저 PDMS 소재로 이루어진 제1고분자보호부(200) 또는 제2고분자보호부(300)를 제조하기 위하여 PDMS와 PDMS 경화제를 10:1의 질량비로 혼합하여 PDMS 용액을 만들수 있다. 설명의 편의상 먼저 제조되는 고분자보호층을 제1고분자보호부(200)이라 정의하며, 이 제1고분자보호부(200)는 도면상 최하층부에 배치되는 것으로 표현될 수 있다.First, in order to manufacture the first polymer protection part 200 or the second polymer protection part 300 made of PDMS material, a PDMS solution can be made by mixing PDMS and PDMS curing agent at a mass ratio of 10:1. For convenience of explanation, the polymer protective layer manufactured first is defined as the first polymer protective portion 200, and this first polymer protective portion 200 can be expressed as being disposed at the lowest layer in the drawing.
제1고분자보호부(200)를 제조하기 위한 PDMS 용액을 회전수단(10)의 선반(20)에 올려놓고 회전수단(10)을 소정 속도로 회전시켜 소정 두께로 얇게 펴는 스핀코팅 공법을 수행한 다음 열 경화를 통해 최종적으로 15~25um(최적치 20um)의 두께를 갖는 유연한 필름 형태로 제작할 수 있다.The PDMS solution for manufacturing the first polymer protection part 200 was placed on the shelf 20 of the rotating means 10, and a spin coating method was performed to spread the PDMS solution to a predetermined thickness by rotating the rotating means 10 at a predetermined speed. Through subsequent heat curing, it can be finally produced in the form of a flexible film with a thickness of 15 to 25 um (optimum 20 um).
계속해서, 제1고분자보호부(200)의 상층부에 색감지부(100)를 제조하기 위하여 PDMS와 PDMS 경화제가 10:1의 질량비로 혼합된 PDMS 용액에 상기 반응 염료(BCG 또는 PR)를 혼합한 후, 이를 제1고분자보호부(200)의 상부에 올려놓고 위와 같은 스핀코팅 공법을 수행할 수 있다.Subsequently, in order to manufacture the color sensing unit 100 on the upper layer of the first polymer protection unit 200, the reactive dye (BCG or PR) was mixed with a PDMS solution in which PDMS and PDMS curing agent were mixed at a mass ratio of 10:1. Afterwards, it can be placed on the top of the first polymer protection part 200 and the spin coating method as above can be performed.
색감지부(100)의 스핀코팅 공법이 끝나면 열 경화를 통해 55~65um(최적치 60um)의 두께를 갖는 유연한 필름 형태의 색감지부(100)가 제1고분자보호부(200)의 상층부에 만들어질 수 있다. After the spin coating method of the color sensing part 100 is completed, the color sensing part 100 in the form of a flexible film with a thickness of 55 to 65 um (optimum 60 um) can be created on the upper layer of the first polymer protection part 200 through heat curing. there is.
마지막으로 색감지부(100)가 제조되고 나면, 색감지부(100)의 상부에 적층되도록 나머지 하나의 제2고분자보호부(300)가 형성될 수 있다.Finally, after the color sensing unit 100 is manufactured, the remaining second polymer protection unit 300 may be formed to be stacked on top of the color sensing unit 100.
제2고분자보호부(300)는 제1고분자보호부(200)와 동일한 조성 및 방법으로 제조되는바, PDMS와 PDMS 경화제의 10:1 질량비로 혼합하여 스핀코팅 공법을 수행하고 열 경화를 통해 15~25um의 두께를 갖는 유연한 필름 형태로 제조될 수 있다.The second polymer protection part 300 is manufactured with the same composition and method as the first polymer protection part 200. PDMS and PDMS curing agent are mixed at a mass ratio of 10:1, spin coating is performed, and heat curing is performed to obtain a 15 It can be manufactured in the form of a flexible film with a thickness of ~25um.
상기한 방법으로 제조된 필름형 색 감지장치의 두께 및 표면 균일성을 confocal microscope를 통해 측정하였는 바, 도 6을 참조하면 대략 60nm의 색감지부(100)와, 각각 대략 20um 두께의 제1고분자보호부(200) 및 제2고분자보호부(300)로 구성된 필름형 색 감지장치의 총 두께는 약 100um의 유연한 필름 형태로 제공될 수 있다.The thickness and surface uniformity of the film-type color sensing device manufactured by the above method were measured using a confocal microscope. Referring to FIG. 6, the color sensing portion 100 of approximately 60 nm and the first polymer protection of approximately 20 μm each were measured. The film-type color sensing device composed of the portion 200 and the second polymer protection portion 300 may be provided in the form of a flexible film with a total thickness of approximately 100 μm.
한편, 이와 같은 방법으로 제조된 필름형 색 감지장치는 중간에 색감지부(100)가 배치되고 그 양측면에 제1고분자보호부(200) 및 제2고분자보호부(300)가 배치되는 3층 레이어(layer) 구조로 제공되는 바, 색감지부(100)의 양측면에 제1고분자보호부(200) 및 제2고분자보호부(300)를 배치한 이유는 PDMS의 기체 투과성과 소수성 특성을 통해 센서의 안정성 및 기체 선택성을 부과하기 위함이다.Meanwhile, the film-type color sensing device manufactured by this method has a three-layer structure in which the color sensing portion 100 is placed in the middle and the first polymer protecting portion 200 and the second polymer protecting portion 300 are disposed on both sides of the color sensing portion 100. It is provided in a (layer) structure, and the reason for arranging the first polymer protection part 200 and the second polymer protection part 300 on both sides of the color sensing part 100 is to protect the sensor through the gas permeability and hydrophobic properties of PDMS. This is to impose stability and gas selectivity.
다시 말해, 색감지부(100)의 상,하부에 소정 두께를 갖는 제1고분자보호부(200) 및 제2고분자보호부(300)를 배치하여도 휘발성 염기 질소 가스의 내부 진입이 가능하므로 색변화를 유발함과 동시에 색감지부(100)에 포함된 반응 염료는 제1고분자보호부(200) 및 제2고분자보호부(300)의 외부로 용출되는 것을 효과적으로 방지할 수 있으므로 반응 염료의 누출에서 높은 안정성을 가질 수 있는 효과가 있다.In other words, even if the first polymer protection part 200 and the second polymer protection part 300 with a predetermined thickness are placed on the upper and lower parts of the color sensing part 100, volatile base nitrogen gas can enter the interior, thereby causing color change. At the same time, it can effectively prevent the reactive dye contained in the color sensing unit 100 from eluting out of the first polymer protection unit 200 and the second polymer protection unit 300, thereby reducing the risk of leakage of the reactive dye. It has the effect of providing stability.
이때, 제1고분자보호부(200) 및 제2고분자보호부(300)의 소수성 특성으로 인한 용액의 불투과성과 PDMS 소재의 높은 가스 투과성으로 인하여 오직 휘발성 염기 질소를 포함하는 염기성 가스의 접촉시에만 색변화를 보이고, 염기성 용액에 노출시에는 소수성 고분자보호층으로 인하여 용액 내 염기성 이온의 침투가 불가능하여 색변화를 보이지 않는 특성을 보이게 된다. 따라서 본 발명의 일 실시예에 따른 필름형 색 감지장치는 염기성 가스인 휘발성 염기 질소에 높은 반응성을 갖는 것을 알 수 있다.At this time, due to the impermeability of the solution due to the hydrophobic nature of the first polymer protection part 200 and the second polymer protection part 300 and the high gas permeability of the PDMS material, only when in contact with basic gas containing volatile base nitrogen. It shows a color change, and when exposed to a basic solution, the basic ions in the solution cannot penetrate due to the hydrophobic polymer protective layer, so it shows no color change. Therefore, it can be seen that the film-type color sensing device according to an embodiment of the present invention has high reactivity to volatile basic nitrogen, which is a basic gas.
상기한 바와 같은 필름형 색 감지장치는 유연성을 가질 뿐만 아니라 도 7에 도시된 바와 같이 우수한 신축성 및 부착성을 갖추고 있기 때문에 다양한 곳(예컨대, 식품 포장재나 용기 등)에 용이하게 적용할 수 있는 장점이 있다. 또한, 필름형 색 감지장치를 휘발성 염기 질소의 일종인 암모니아 가스에 노출시켰을 때 노란색이 파란색으로 색변화하는 것을 확인할 수 있으므로, 사용자의 육안 확인성을 높일 수 있다.The film-type color sensing device as described above is not only flexible, but also has excellent elasticity and adhesion as shown in FIG. 7, so it can be easily applied to various places (e.g., food packaging materials or containers, etc.) There is. In addition, when a film-type color sensing device is exposed to ammonia gas, a type of volatile basic nitrogen, it can be confirmed that the color changes from yellow to blue, thereby improving the user's visual confirmation.
참고로, 도 8에 도시된 바와 같이 필름형 색 감지장치가 암모니아 가스에 노출시 흡광도가 약 460nm에서 감소하고 628nm 영역에서 증가하는 것을 확인할 수 있으며, 암모니아 기체로 인해 색감지부(100)가 제1고분자보호부(200) 및 제2고분자보호부(300)의 내부에서도 효율적으로 탈수소화 반응이 일어나고 공명 안정성을 갖는 것을 확인할 수 있다.For reference, as shown in FIG. 8, it can be seen that when the film-type color sensing device is exposed to ammonia gas, the absorbance decreases at about 460 nm and increases in the 628 nm region, and the color sensing unit 100 is first exposed to the ammonia gas. It can be confirmed that the dehydrogenation reaction occurs efficiently inside the polymer protection unit 200 and the second polymer protection unit 300 and has resonance stability.
또한 암모니아 기체의 농도가 약 50ppm 이상으로 증가하면 육안으로 색 변화가 감지될 뿐만 아니라, 628nm 영역의 흡광도 증가가 암모니아 기체 농도에 따라 선형적으로 증가하는 것을 확인할 수 있다.Additionally, when the concentration of ammonia gas increases to about 50ppm or more, not only can a color change be detected with the naked eye, but it can also be seen that the increase in absorbance in the 628 nm region increases linearly according to the ammonia gas concentration.
따라서, 배경기술에서 언급한 바와 같이 노동자의 암모니아 가스 노출이 8시간 동안 약 50ppm 이하로 되어야 하며, 육류 및 어패류의 부패로 인하여 발생하는 휘발성 염기 질소 기체의 농도가 약 20mg/100g (약 200ppm) 영역이기 때문에 본 실시예에 따른 필름형 색 감지장치의 경우 다양한 산업 분야 및 식품 분야에 용이하게 적용 가능한 장점이 있다.Therefore, as mentioned in the background technology, workers' exposure to ammonia gas should be less than about 50ppm for 8 hours, and the concentration of volatile base nitrogen gas generated from rotting meat and fish and shellfish should be in the range of about 20mg/100g (about 200ppm). Therefore, the film-type color sensing device according to this embodiment has the advantage of being easily applicable to various industrial and food fields.
한편, 본 발명의 일 실시예에 따른 필름형 색 감지장치의 범용성을 증명하기 위해 아래와 같은 응용 연구를 수행하였다.Meanwhile, the following application research was conducted to prove the versatility of the film-type color sensing device according to an embodiment of the present invention.
도 9를 참조하면, 산업 현장에서 암모니아 가스 누출을 검출하기 위해 본 실시예에 따른 필름형 색 감지장치를 안전 헬멧에 부착하고 암모니아 가스에 노출 실험을 수행하였는 바, 도 9에 도시된 바와 같이 안전 헬멧 상에 부착된 색감지부(100)의 색이 노랑색에서 파랑색으로 색변화함으로써 암모니아 가스에 노출됨을 손쉽게 확인할 수 있다.Referring to FIG. 9, in order to detect ammonia gas leakage at industrial sites, the film-type color detection device according to this embodiment was attached to a safety helmet and an exposure experiment to ammonia gas was performed. As shown in FIG. 9, safety Exposure to ammonia gas can be easily confirmed by changing the color of the color sensing unit 100 attached to the helmet from yellow to blue.
이 실험에 따르면 암모니아 약 50ppm 이상의 농도에 약 3분간 노출되었을 때 색변화를 육안으로 확인할 수 있을 뿐만 아니라, 흡광도(628nm)의 경우도 암모니아 가스 농도의 증가에 따라 증가함을 확인할 수 있다.According to this experiment, not only can a color change be confirmed with the naked eye when exposed to an ammonia concentration of about 50 ppm or more for about 3 minutes, but also the absorbance (628 nm) can be confirmed to increase as the ammonia gas concentration increases.
또한, 도 10을 참조하면 식품 산업에서 응용 가능성을 확인하기 위해 rochfish(볼락) 샘플을 채취하여 상온에서 약 20시간 보관하여 색변화를 관찰하였는 바, 도 10에 도시된 바와 같이 식품이 부패하였을 때 색감지부(100)가 노란색에서 파란색으로 색변화하는 것을 확인할 수 있다.In addition, referring to Figure 10, in order to confirm applicability in the food industry, rochfish (rockfish) samples were collected and stored at room temperature for about 20 hours to observe color change. As shown in Figure 10, when the food spoiled, It can be seen that the color sensing unit 100 changes color from yellow to blue.
한편, urease-생산 미생물을 색센서를 이용하여 검출하기 위하여 도 11에 도시된 urea가 포함된 agar medium을 제작하고 효소 및 미생물 실험을 진행하였다.Meanwhile, in order to detect urease-producing microorganisms using a color sensor, an agar medium containing urea shown in Figure 11 was prepared and enzyme and microorganism experiments were performed.
이를 통해, medium 내에 포함된 urea와 urease 간의 hydrolysis 반응을 통하여 암모니아가 형성되며 이를 본 실시예에 따른 필름형 색 감지장치로 검출할 수 있는 바, urease의 농도에 따라 암모니아 배출 정도가 증가하는 것을 확인할 수 있다.Through this, ammonia is formed through a hydrolysis reaction between urea and urease contained in the medium, and this can be detected with the film-type color detection device according to this embodiment, confirming that the degree of ammonia emission increases depending on the concentration of urease. You can.
이러한 결과를 바탕으로 urea가 포함된 agar medium에 도 12의 표와 같이 다양한 미생물을 대상으로 urease-생산 미생물을 본 실시예에 따른 필름형 색 감지장치를 이용하여 검출할 수 있다.Based on these results, urease-producing microorganisms can be detected for various microorganisms in agar medium containing urea as shown in the table in FIG. 12 using the film-type color detection device according to this embodiment.
또한, 색감지부(100)의 색변화가 미생물의 urease 생성과 관련이 있음을 증명하기 위해 urease를 저해하는 inhibitor를 사용하여 색변화를 확인하였다.In addition, in order to prove that the color change of the color sensing unit 100 is related to the production of urease by microorganisms, the color change was confirmed using an inhibitor that inhibits urease.
PPDA(phenyl phosphorodiamidate)로 처리된 미생물은 12간의 배양에도 불구하고 색변화를 관찰할 수 없었으나, PPDA로 처리되지 않은 미생물은 약 6시간 후부터 색변화를 확인할 수 있었다.For microorganisms treated with PPDA (phenyl phosphorodiamidate), no color change could be observed despite culturing for 12 hours, but for microorganisms not treated with PPDA, color change could be observed after about 6 hours.
이는 필름형 색 감지장치의 색변화가 미생물의 urease 생성으로 인한 것임을 증명하는 것으로, 본 발명은 urease 생성 미생물의 검출 및 진단에 응용 가능하다.This proves that the color change of the film-type color detection device is due to urease production by microorganisms, and the present invention is applicable to the detection and diagnosis of urease-producing microorganisms.
한편, 본 발명의 일 실시예에 따른 필름형 색 감지장치의 재사용성을 확인하기 위해 휘발성 염기 질소 기체와 반응하여 색이 변한 필름형 색 감지장치를 아세트산 기체 혹은 공기 중에 노출하여 재현성을 확인하였다.Meanwhile, in order to confirm the reusability of the film-type color sensing device according to an embodiment of the present invention, the film-type color sensing device whose color changed by reacting with volatile base nitrogen gas was exposed to acetic acid gas or air to confirm reproducibility.
그 결과, 도 13에 도시된 바와 같이 아세트산 기체에 노출시 약 10분 이내에 원래 상태인 노란색으로 회복되는 것을 확인할 수 있었다. 또한, 약 24시간 공기 노출을 통해 색이 원래 상태인 노란색으로 회복하는 것을 확인할 수 있었다.As a result, as shown in Figure 13, it was confirmed that the original yellow color was restored within about 10 minutes when exposed to acetic acid gas. In addition, it was confirmed that the color returned to its original yellow state through air exposure for about 24 hours.
구체적으로, 본 발명의 일 실시예에 따른 필름형 색 감지장치의 재활용성을 테스트하기 위해 아래와 같이 2 종류의 실험(급속 탈착 및 저속 탈착)을 진행하였다.Specifically, to test the recyclability of the film-type color sensing device according to an embodiment of the present invention, two types of experiments (rapid desorption and slow desorption) were conducted as follows.
1. acetic acid fume 5초간 노출 또는 0.1 N acetic acid 용액에 2시간 담지(급속 탈착 실험)1. Exposure to acetic acid fume for 5 seconds or immersion in 0.1 N acetic acid solution for 2 hours (rapid desorption experiment)
- Acetic acid (1N)의 액체에서 발생되는 fume에 5초간 노출하여 흡착된 암모니아 가스 유도체와의 중화반응을 유도하였으며, 5초의 노출에서 색 감지장치는 노출전 색으로 복귀하는 것을 확인할 수 있었다.- A neutralization reaction with the adsorbed ammonia gas derivative was induced by exposure to fume generated from acetic acid (1N) liquid for 5 seconds, and it was confirmed that the color detection device returned to the color before exposure at 5 seconds of exposure.
- 암모니아 반응을 통해 파란색으로 변한 소재를 0.05~0.1N 아세트산 용액에 약 1~2시간 담지하여 암모니아와 아세트산 간의 중화반응 유도 진행하였으며, 노출후 색 감지장치는 노출전 색으로 복귀하는 것을 확인할 수 있었다.- The material that had turned blue through the ammonia reaction was placed in a 0.05-0.1N acetic acid solution for about 1-2 hours to induce a neutralization reaction between ammonia and acetic acid, and it was confirmed that the color detection device returned to the color before exposure after exposure. .
2. ammonia-free 상태의 공기중에 24~48시간 방치하여 확산에 의한 자연 탈착 진행(저속 탈착 실험)2. Natural desorption through diffusion by leaving in ammonia-free air for 24 to 48 hours (low-speed desorption experiment)
- 암모니아 반응을 통해 파란색으로 변한 소재를 암모니아 노출이 없는 공기중에 약 24~48시간 노출시 암모니아 기체는 공기 중으로 확산이 일어나는 바, 이에 따라 원래 색으로 복귀하는 것을 확인할 수 있었다.- When the material that had turned blue through the ammonia reaction was exposed to air without ammonia for about 24 to 48 hours, the ammonia gas diffused into the air, and it was confirmed that it returned to its original color.
한편 도 14를 참조하면, 본 발명의 다른 실시예에 따른 필름형 색 감지장치는 색감지층(400) 및 보호층(500)을 포함할 수 있다.Meanwhile, referring to FIG. 14, a film-type color sensing device according to another embodiment of the present invention may include a color sensing layer 400 and a protective layer 500.
본 발명의 다른 실시예에 따른 필름형 색 감지장치는 앞에서 설명한 필름형 색 감지장치와 달리 스프레이 공법에 의해 식품용 키친랩과 같은 식품용 수지재(30)에 코팅되는 것으로, 제조 공법에 차이가 있으며, 식품용 수지재(30)에 도포되므로 하나의 보호층(500)만 필요하여 총 2층 구조를 갖게 되는 차이점 이외에는 본 발명의 일 실시예와 기본적으로 메커니즘과 동일한 실험 결과 및 효과를 갖는다.Unlike the film-type color sensing device described above, the film-type color sensing device according to another embodiment of the present invention is coated on a food resin material 30, such as kitchen wrap for food, by a spray method, and there is a difference in the manufacturing method. In addition, since it is applied to the food resin material 30, only one protective layer 500 is required, resulting in a total two-layer structure, and has basically the same experimental results and effects as the mechanism of one embodiment of the present invention.
색감지층(400)은 상기한 색감지부(100)와 기본적으로 동일한 구성으로서 스프레이 방식에 의해 도포된 층을 의미할 수 있다. 따라서, 색감지층(400)은 염기성 가스에 반응하여 색 변화가 발생하도록 소정의 반응 염료를 포함하며, 식품용 수지재(30)의 표면 상에 소정 두께의 층 형상으로 제공될 수 있다.The color-sensing layer 400 has basically the same structure as the color-sensing unit 100 described above and may refer to a layer applied by a spray method. Accordingly, the color-sensing layer 400 contains a predetermined reactive dye so that a color change occurs in response to a basic gas, and may be provided in the form of a layer with a predetermined thickness on the surface of the food resin material 30.
여기서, 반응 염료는 pH 지시약 상용 염료로서, pH 4~8 사이에서 색변화를 갖는 Bromocresol green(BCG), phenol red(PR), methyl orange(MO), methyl red(MR), litmus, methyle purple(MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein 및 universal indicator 중 어느 하나가 사용될 수 있다.Here, the reactive dyes are commercially available pH indicator dyes, including bromocresol green (BCG), phenol red (PR), methyl orange (MO), methyl red (MR), litmus, and methyle purple ( Any one of MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and universal indicator can be used.
색감지층(400)은 PDMS용액에 반응 염료를 혼합하여 교반한 후 hexane용액을 사용하여 희석하고, 이를 스프레이 공법을 수행하여 식품용 수지재(30)에 도포한 후 열처리하는 과정을 통하여 소정 두깨를 갖는 코팅층 형태로 제공될 수 있다.The color-sensing layer 400 is made by mixing a reactive dye in a PDMS solution, stirring it, diluting it using a hexane solution, applying it to the food resin material 30 using a spray method, and then heat-treating it to obtain a predetermined thickness. It may be provided in the form of a coating layer having a coating layer.
구체적으로, 색감지층(400)은 아래와 같은 방법에 의해 제조될 수 있다.Specifically, the color-sensing layer 400 can be manufactured by the following method.
약 70mg/ml의 반응 염료 용액 500ul를 약 5g의 PDMS용액에 담지(혼합)하여 22~26시간 100~300rpm에서 교반하고, 효율적인 스프레이를 위해 약 15g의 hexane 용액을 사용하여 2차 희석(25wt% BCG-PDMS/Hexane)을 진행한다. 이렇게 제작된 용액은 스프레이 장치를 통하여 약 35~45psi의 압력으로 식품용 수지재(30)의 표면에서 25~35cm의 거리를 두고 150~250um 노즐을 통해 3~5초간 스프레이 도포하며, 도포후 1~3분간 55~65 ℃에서 열처리함으로써 색감지층(400)을 제조할 수 있다.500ul of a reactive dye solution of about 70mg/ml was placed (mixed) in about 5g of PDMS solution and stirred at 100~300rpm for 22~26 hours. For efficient spraying, a second dilution (25wt%) was made using about 15g of hexane solution. BCG-PDMS/Hexane) is performed. The solution produced in this way is sprayed for 3 to 5 seconds through a 150 to 250 um nozzle at a distance of 25 to 35 cm from the surface of the food resin material 30 at a pressure of about 35 to 45 psi through a spray device. After application, 1 The color-sensing layer 400 can be manufactured by heat treatment at 55-65°C for ~3 minutes.
또한, 상기 보호층(500)은 상기 제1고분자보호부(200) 또는 상기 제2고분자보호부(300)와 유사한 구성으로서, 식품용 수지재(30)의 반대측에 해당하는 색감지부(100)의 일측면에 적층되며, 염기성 가스는 투과시키고 반응 염료의 누출은 방지하기 위해 소수성 및 투과성을 갖는 PDMS소재로 제공될 수 있다.In addition, the protective layer 500 has a similar structure to the first polymer protection part 200 or the second polymer protection part 300, and has a color sensing part 100 corresponding to the opposite side of the food resin material 30. It is laminated on one side and can be made of PDMS material with hydrophobicity and permeability to allow basic gas to pass through and to prevent leakage of reactive dye.
여기서, 보호층(500)은 PDMS와 PDMS 경화제가 혼합된 PDMS용액을 스프레이 공법을 통하여 색감지층(400)의 표면상에 도포한 후 소정 조건에서 열처리함으로써 색감지층(400)을 감싸는 코팅층 형태로 제공될 수 있다.Here, the protective layer 500 is provided in the form of a coating layer surrounding the color-sensing layer 400 by applying a PDMS solution mixed with PDMS and PDMS curing agent on the surface of the color-sensing layer 400 through a spray method and then heat-treating it under predetermined conditions. It can be.
구체적으로, 보호층(500)은 PDMS용액을 35~45 psi의 압력으로 색감지층(400)의 표면에서 25~35cm의 거리를 두고 3~5초간 스프레이 도포하고, 도포후 1~3분간 55~65 ℃에서 열처리함으로써 제조될 수 있다.Specifically, the protective layer 500 is spray-applied with a PDMS solution at a pressure of 35-45 psi for 3-5 seconds at a distance of 25-35 cm from the surface of the color-sensing layer 400, and then applied at a pressure of 55-45 psi for 1-3 minutes. It can be prepared by heat treatment at 65°C.
즉, 본 발명의 다른 실시예에 의한 필름형 색 감지장치는 식품용 키친랩과 같은 식품용 수지재(30)에 스프레이 공법을 통해 색감지층(400) 및 보호층(500)을 차례대로 적층 코팅함으로써 보호층이 한 개 감소된 2층 구조의 박막 형태로 제조할 수 있는데, 스프레이 코팅방법에 의하더라도 앞에서 설명한 3층 구조의 본 발명의 일 실시예와 효과 및 실험 결과는 동일한 것을 확인할 수 있었다. That is, the film-type color sensing device according to another embodiment of the present invention sequentially laminates and coats the color sensing layer 400 and the protective layer 500 on a food resin material 30, such as kitchen wrap for food, through a spray method. By doing so, it can be manufactured in the form of a two-layer thin film with one reduced protective layer, and it was confirmed that the effects and experimental results are the same as those of an embodiment of the present invention with a three-layer structure described above even by the spray coating method.
이상 본 발명의 실시예에 따른 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치 및 그 제조방법을 구체적인 실시 형태로서 설명하였으나, 이는 예시에 불과한 것으로서 본 발명은 이에 한정되지 않는 것이며, 본 명세서에 개시된 기초 사상에 따르는 최광의 범위를 갖는 것으로 해석되어야 한다. 당업자는 개시된 실시 형태들을 조합, 치환하여 적시되지 않은 실시 형태를 실시할 수 있으나, 이 역시 본 발명의 권리범위를 벗어나지 않는 것이다. 이외에도 당업자는 본 명세서에 기초하여 개시된 실시형태를 용이하게 변경 또는 변형할 수 있으며, 이러한 변경 또는 변형도 본 발명의 권리범위에 속함은 명백하다.Above, the film-type color sensing device for detecting volatile basic nitrogen gas according to an embodiment of the present invention and its manufacturing method have been described as specific embodiments, but this is only an example and the present invention is not limited thereto, and the disclosure disclosed herein It should be interpreted as having the widest scope according to the basic idea. A person skilled in the art may combine and substitute the disclosed embodiments to implement embodiments not specified, but this also does not deviate from the scope of the present invention. In addition, a person skilled in the art can easily change or modify the embodiments disclosed based on the present specification, and it is clear that such changes or modifications also fall within the scope of the present invention.
본 발명은 휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치 및 그 제조방법에 관한 것으로서, 산업상 이용 가능하다.The present invention relates to a film-type color sensing device for detecting volatile basic nitrogen gas and a method of manufacturing the same, and can be used industrially.
Claims (17)
- 염기성 가스에 반응하여 색 변화가 발생하도록 소정의 반응 염료를 포함하며, 소정 두께의 층(layer) 형상으로 제공되는 색감지부;A color sensing unit containing a predetermined reactive dye to cause a color change in response to a basic gas and provided in the form of a layer with a predetermined thickness;상기 색감지부를 사이에 두고 그 일측면에 적층되며, 상기 염기성 가스는 투과시키고 상기 반응 염료의 누출은 방지하기 위해 소수성 및 기체 투과성을 갖는 PDMS 소재로 제공되는 제1고분자보호부; 및A first polymer protection part laminated on one side of the color sensing part with the color sensing part in between, and made of PDMS material having hydrophobicity and gas permeability to transmit the basic gas and prevent leakage of the reactive dye; and상기 색감지부를 사이에 두고 그 타측면에 적층되며, 상기 염기성 가스는 투과시키고 상기 반응 염료의 누출은 방지하기 위해 소수성 및 기체 투과성을 갖는 PDMS 소재로 제공되는 제2고분자보호부;를 포함하는,A second polymer protection part is laminated on the other side of the color sensing part with the color sensing part in between, and is made of PDMS material having hydrophobicity and gas permeability to transmit the basic gas and prevent leakage of the reactive dye.휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제1 항에 있어서,According to claim 1,상기 염기성 가스는 휘발성 염기 질소인 것을 특징으로 하는,Characterized in that the basic gas is volatile basic nitrogen,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제1 항에 있어서,According to claim 1,상기 반응 염료는 pH 지시약 상용 염료로서, pH 4~8 사이에서 색변화를 갖는 Bromocresol green(BCG), phenol red(PR), methyl orange(MO), methyl red(MR), litmus, methyle purple(MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein 및 universal indicator 중 어느 하나가 사용된 것을 특징으로 하는, The reactive dyes are commercial pH indicator dyes, including bromocresol green (BCG), phenol red (PR), methyl orange (MO), methyl red (MR), litmus, and methyle purple (MP), which change color between pH 4 and 8. ), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and universal indicator,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제3 항에 있어서,According to clause 3,상기 색감지부는 PDMS와 PDMS 경화제가 10:1의 질량비로 혼합된 PDMS용액에 상기 반응 염료를 혼합하고 스핀코팅 공법을 수행한 후 열 경화를 통해 55~65um의 두께를 갖는 유연한 필름 형태로 제공되는 것을 특징으로 하는, The color sensing unit is provided in the form of a flexible film with a thickness of 55 to 65 um through heat curing by mixing the reactive dye with a PDMS solution in which PDMS and PDMS curing agent are mixed at a mass ratio of 10:1, performing a spin coating method, and then heat curing. Characterized by휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제1 항에 있어서,According to claim 1,상기 제1고분자보호부 및 상기 제2고분자보호부는 PDMS와 PDMS 경화제를 10:1의 질량비로 혼합하여 스핀코팅 공법을 수행하고 열경화를 통해 15~25um의 두께를 갖는 유연한 필름 형태로 제공되는 것을 특징으로 하는, The first polymer protective part and the second polymer protective part are provided in the form of a flexible film with a thickness of 15 to 25 um through spin coating by mixing PDMS and PDMS curing agent at a mass ratio of 10:1 and thermal curing. Characterized by,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- PDMS와 PDMS경화제를 10:1의 질량비로 혼합하여 PDMS용액을 만드는 단계;Making a PDMS solution by mixing PDMS and PDMS curing agent at a mass ratio of 10:1;상기 PDMS용액을 회전수단에 올려 놓고 소정 속도로 회전시켜 소정 두께로 펴는 스핀코팅 공법을 수행하고, 열 경화를 통해 유연한 필름 형태의 제1고분자보호부를 형성하는 단계;Performing a spin coating method of placing the PDMS solution on a rotating means and rotating it at a predetermined speed to spread it to a predetermined thickness, and forming a first polymer protection part in the form of a flexible film through heat curing;PDMS와 PDMS경화제가 10:1의 질량비로 혼합된 PDMS용액에 반응 염료를 혼합한 후 이를 상기 제1고분자보호부의 상부에 올려놓고 스핀코팅 공법을 수행하고 열 경화를 통해 상기 제1고분자보호부의 상부에 유연한 필름 형태의 색감지부를 형성하는 단계; 및After mixing the reactive dye with the PDMS solution in which PDMS and PDMS curing agent are mixed at a mass ratio of 10:1, it is placed on the top of the first polymer protective part, a spin coating process is performed, and the upper part of the first polymer protective part is formed through heat curing. forming a color sensing unit in the form of a flexible film; and상기 PDMS용액을 상기 색감지부의 상부에 올려 놓고 스핀코팅 공법을 수행한 후 열 경화를 통해 상기 색감지부의 상부에 유연한 필름 형태의 제2고분자보호부를 형성하는 단계;를 포함하는,Placing the PDMS solution on top of the color sensing unit, performing a spin coating method, and then forming a second polymer protection part in the form of a flexible film on the upper part of the color sensing unit through heat curing; comprising,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법.Method for manufacturing a film-type color sensing device for detecting volatile basic nitrogen gas.
- 제6 항에 있어서,According to clause 6,상기 제1고분자보호부 및 상기 제2고분자보호부는 15~25um의 두께를 가지고,The first polymer protection part and the second polymer protection part have a thickness of 15 to 25 um,상기 색감지부는 55~65um의 두께를 갖도록 제조되는 것을 특징으로 하는, Characterized in that the color sensing unit is manufactured to have a thickness of 55 to 65 um.휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법.Method for manufacturing a film-type color sensing device for detecting volatile basic nitrogen gas.
- 염기성 가스에 반응하여 색 변화가 발생하도록 소정의 반응 염료를 포함하며, 식품용 수지재의 표면 상에 소정 두께의 층(layer) 형상으로 제공되는 색감지층; 및A color-sensing layer containing a predetermined reactive dye so that a color change occurs in response to a basic gas, and provided in the form of a layer of a predetermined thickness on the surface of the food resin material; and상기 식품용 수지재의 반대측에 해당하는 상기 색감지부의 일측면에 적층되며, 상기 염기성 가스는 투과시키고 상기 반응 염료의 누출은 방지하기 위해 소수성 및 기체 투과성을 갖는 PDMS 소재로 제공되는 보호층;을 포함하는,A protective layer is laminated on one side of the color sensing unit corresponding to the opposite side of the food resin material and is made of a hydrophobic and gas-permeable PDMS material to transmit the basic gas and prevent leakage of the reactive dye. doing,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제8 항에 있어서,According to clause 8,상기 염기성 가스는 휘발성 염기 질소인 것을 특징으로 하는,Characterized in that the basic gas is volatile basic nitrogen,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제8 항에 있어서,According to clause 8,상기 반응 염료는 pH 지시약 상용 염료로서, pH 4~8 사이에서 색변화를 갖는 Bromocresol green(BCG), phenol red(PR), methyl orange(MO), methyl red(MR), litmus, methyle purple(MP), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein 및 universal indicator 중 어느 하나가 사용된 것을 특징으로 하는, The reactive dyes are commercial pH indicator dyes, including bromocresol green (BCG), phenol red (PR), methyl orange (MO), methyl red (MR), litmus, and methyle purple (MP), which change color between pH 4 and 8. ), bromcresol purple, bromthymol blue, neutral red, phenol red, phenolphthalein, and universal indicator,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제8 항에 있어서,According to clause 8,상기 색감지층은 PDMS용액에 상기 반응 염료를 혼합하여 교반한 후 hexane 용액을 사용하여 희석하고, 이를 스프레이 공법을 수행하여 상기 식품용 수지재에 도포한 후 소정 조건에서의 열처리하는 과정을 통하여 코팅층 형태로 제공되는 것을 특징으로 하는,The color-sensing layer is formed by mixing and stirring the reactive dye in the PDMS solution, diluting it using a hexane solution, applying it to the food resin material by spraying it, and then heat-treating it under predetermined conditions to form a coating layer. Characterized in that it is provided as,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제11 항에 있어서,According to claim 11,상기 색감지층은, 상기 PDMS용액에 상기 반응염료를 혼합하여 22~26시간 100~300rpm에서 교반하고, hexane용액을 사용하여 희석하고 나면, 35~45psi의 압력으로 상기 식품용 수지재의 표면에서 25~35cm의 거리를 두고 150~250um 노즐을 통해 3~5초간 스프레이 도포하며, 도포후 1~3분간 55~65 ℃에서 열처리하는 것을 특징으로 하는,The color-sensing layer is formed by mixing the reactive dye in the PDMS solution, stirring at 100-300 rpm for 22-26 hours, and diluting it with a hexane solution, and then forming the reaction dye on the surface of the food resin material at a pressure of 35-45 psi. Characterized by spraying for 3 to 5 seconds through a 150 to 250 um nozzle at a distance of 35 cm and heat treating at 55 to 65 ° C for 1 to 3 minutes after application.휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제11 항 또는 제12 항에 있어서,The method of claim 11 or 12,상기 보호층은 PDMS와 PDMS 경화제가 혼합된 PDMS용액을 스프레이 공법을 통하여 상기 색감지층의 표면상에 도포한 후 소정 조건에서 열처리하는 과정을 통하여 상기 색감지층을 감싸는 코팅층 형태로 제공되는 것을 특징으로 하는, The protective layer is provided in the form of a coating layer surrounding the color-sensing layer by applying a PDMS solution mixed with PDMS and PDMS curing agent on the surface of the color-sensing layer through a spray method and then heat-treating it under predetermined conditions. ,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- 제13 항에 있어서,According to claim 13,상기 보호층은 상기 PDMS용액을 35~45psi의 압력으로 상기 색감지층의 표면에서 25~35cm의 거리를 두고 3~5초간 스프레이 도포하고, 도포 후 1~3분간 55~65 ℃에서 열처리하는 것을 특징으로 하는,The protective layer is characterized in that the PDMS solution is spray-applied at a pressure of 35-45 psi for 3-5 seconds at a distance of 25-35 cm from the surface of the color-sensing layer, and heat-treated at 55-65 ° C for 1-3 minutes after application. to,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치.Film-type color detection device for detecting volatile basic nitrogen gas.
- PDMS용액에 반응 염료를 혼합하여 교반한 후 hexane용액을 사용하여 희석한 다음 이를 소정 압력으로 식품용 수지재의 표면 상에 스프레이 도포하는 단계;Mixing and stirring a reactive dye in the PDMS solution, diluting it with a hexane solution, and then spraying it onto the surface of the food resin material at a predetermined pressure;스프레이 도포 후 소정 조건에서 열처리하여 코팅층 형태의 색감지층을 형성하는 단계;Forming a color-sensitive layer in the form of a coating layer by heat-treating it under predetermined conditions after spray application;상기 색감지층이 형성된 후 PDMS용액을 상기 색감지층의 표면상에 도포하는 단계; 및After the color-sensing layer is formed, applying a PDMS solution onto the surface of the color-sensing layer; and상기 PDMS용액을 도포한 후 소정 조건에서 열처리하여 상기 색감지층을 감싸는 코팅층 형태의 보호층을 형성하는 단계;를 포함하는,Comprising: applying the PDMS solution and then heat-treating it under predetermined conditions to form a protective layer in the form of a coating layer surrounding the color-sensing layer;휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법.Method for manufacturing a film-type color sensing device for detecting volatile basic nitrogen gas.
- 제15 항에 있어서,According to claim 15,상기 색감지층은, 상기 PDMS용액에 상기 반응염료를 혼합하여 22~26시간, 100~300rpm에서 교반하고, hexane용액을 사용하여 희석하고 나면, 35~45psi의 압력으로 상기 식품용 수지재의 표면에서 25~35cm의 거리를 두고 150~250um 노즐을 통해 3~5초간 스프레이 도포하며, 도포후 1~3분간 55~65 ℃에서 열처리하는 것을 특징으로 하는,The color-sensing layer is formed by mixing the reactive dye in the PDMS solution, stirring it at 100-300 rpm for 22-26 hours, and diluting it with a hexane solution, and then 25 psi on the surface of the food resin material at a pressure of 35-45 psi. Characterized by spraying for 3 to 5 seconds through a 150 to 250um nozzle at a distance of ~35cm and heat treating at 55 to 65 ℃ for 1 to 3 minutes after application.휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법.Method for manufacturing a film-type color sensing device for detecting volatile basic nitrogen gas.
- 제16 항에 있어서,According to claim 16,상기 보호층은 상기 PDMS용액을 35~45psi의 압력으로 상기 색감지층의 표면에서 25~35cm의 거리를 두고 3~5초간 스프레이 도포하고, 도포 후 1~3분간 55~65 ℃에서 열처리하는 것을 특징으로 하는,The protective layer is characterized in that the PDMS solution is spray-applied at a pressure of 35-45 psi for 3-5 seconds at a distance of 25-35 cm from the surface of the color-sensing layer, and heat-treated at 55-65 ° C for 1-3 minutes after application. to,휘발성 염기질소 가스 검출을 위한 필름형 색 감지장치의 제조방법. Method for manufacturing a film-type color sensing device for detecting volatile basic nitrogen gas.
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| KR1020230061322A KR20240023368A (en) | 2022-08-12 | 2023-05-11 | Colorimetric film sensing device for detection of total volatile basic nitrogen and manufacturing method thereof |
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| US20030159928A1 (en) * | 2002-02-28 | 2003-08-28 | Ngk Spark Plug Co., Ltd. | Prismatic ceramic heater for heating gas sensor element, prismatic gas sensor element in multilayered structure including the prismatic ceramic heater, and method for manufacturing the prismatic ceramic heater and prismatic gas sensor element |
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| KR20190121897A (en) * | 2018-04-18 | 2019-10-29 | 동국대학교 산학협력단 | Fressness indicator |
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| US20030159928A1 (en) * | 2002-02-28 | 2003-08-28 | Ngk Spark Plug Co., Ltd. | Prismatic ceramic heater for heating gas sensor element, prismatic gas sensor element in multilayered structure including the prismatic ceramic heater, and method for manufacturing the prismatic ceramic heater and prismatic gas sensor element |
| KR20090010640A (en) * | 2007-07-24 | 2009-01-30 | 한국과학기술원 | Apparatus and method for monitoring a gas using gas - permeable material |
| KR102412393B1 (en) * | 2017-02-17 | 2022-06-22 | 닛토덴코 가부시키가이샤 | gas sensing element |
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