KR20180134149A - Hydrogen-detecting sensor, method of forming the hydrogen-detecting sensor, and hydrogen-detecting miscellaneous goods - Google Patents

Hydrogen-detecting sensor, method of forming the hydrogen-detecting sensor, and hydrogen-detecting miscellaneous goods Download PDF

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KR20180134149A
KR20180134149A KR1020170071659A KR20170071659A KR20180134149A KR 20180134149 A KR20180134149 A KR 20180134149A KR 1020170071659 A KR1020170071659 A KR 1020170071659A KR 20170071659 A KR20170071659 A KR 20170071659A KR 20180134149 A KR20180134149 A KR 20180134149A
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South Korea
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hydrogen
hydrogen sensing
based support
solution
sensing
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KR1020170071659A
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Korean (ko)
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KR101990120B1 (en
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김서영
박성훈
장예원
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하이리움에너지 주식회사
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Priority to KR1020170071659A priority Critical patent/KR101990120B1/en
Priority to PCT/KR2017/008819 priority patent/WO2018225894A1/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/08—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of metallic material
    • 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
    • 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
    • G01N21/783—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 for analysing gases
    • 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
    • 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
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—Specially adapted to detect a particular component
    • G01N33/005—Specially adapted to detect a particular component for H2

Abstract

The present invention relates to a hydrogen sensing device comprising a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, and a plurality of titanium-based support particles and a plurality of platinum group-based oxides respectively disposed on the plurality of tungsten- ; And silicon compounded with the hydrogen sensing pigment.

Description

TECHNICAL FIELD [0001] The present invention relates to a hydrogen sensor, a method of manufacturing the hydrogen sensor, and a hydrogen sensing material. BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a hydrogen sensor,

The present invention relates to a hydrogen detection sensor suitable for detecting hydrogen gas leaking into the air from at least one of an outer wall of a hydrogen reaction apparatus or a hydrogen production apparatus and a hydrogen supply apparatus or a hydrogen supply apparatus, A method of manufacturing a hydrogen sensor, and a hydrogen sensing article.

Recently, due to the continuous use of fossil fuels, energy supply and demand due to depletion of fossil fuels has been rising all over the world. Development of clean energy resources is focused on hydrogen that can be easily obtained from water as an alternative to solve the energy supply and demand problem.

Hydrogen energy is an alternative to solve global warming, so it shows a great potential for future development. As a result, hydrogen energy development is proceeding at a rapid pace. However, since gas has kinetic energy greater than liquid and solid, there is always a risk of gas leakage from a reaction apparatus using gas or a manufacturing apparatus manufacturing gas.

Particularly, hydrogen in the gas easily spreads from the reaction device or the production device of the hydrogen gas during the aging of the reaction device or the production device of the hydrogen gas since the hydrogen gas has a very high molecular motion speed and is easily diffused.

In addition, since the leaked hydrogen has a lower explosion limit of about 4% in air, the leaked hydrogen and oxygen mixed gas often cause oxygen hydrogen explosive gas reaction, Or cause human accidents.

Therefore, in order for the hydrogen to be widely used as clean energy, the hydrogen must be easily detected even when it leaks into the air from the reaction apparatus or the production apparatus in a small amount. In this case, the leakage of the hydrogen into the air is detected by the hydrogen sensor or the hydrogen detection sensor in the prior art.

A prior art hydrogen sensor is disclosed in Korean Patent Laid-Open Publication No. 10-2012-0088409. The hydrogen sensor is formed by etching a silicon substrate to a predetermined depth and protruding a plurality of 'rough Si' nanowires from the etched silicon substrate and depositing palladium (Pd) on a plurality of 'rough Si' nanowires.

Here, since the hydrogen sensor uses a silicon substrate, the hydrogen sensor has low physical properties, for example, hardness of the substrate, occupied area of the substrate, or low flexibility in use due to the structure of the substrate.

Further, since the hydrogen sensor detects hydrogen by contact between clusters (= nanowire lumps) in a plurality of 'rough Si' nanowires and expansion of palladium, it is difficult to detect the entire range of hydrogen concentration in the air in a short time . A conventional hydrogen detection sensor is disclosed in Korean Patent Laid-Open Publication No. 10-2006-0070749.

The hydrogen sensing sensor is formed by forming a palladium pattern partially exposed in air on an SOI substrate and connecting an electric wire to a palladium pattern and an SOI substrate, respectively. Since the hydrogen sensing sensor is driven by applying power from the outside to the MOS structure formed on the SOI substrate, it is used only around the power supply, so that the degree of freedom of use is small, which is low applicability.

In addition, since the hydrogen sensing sensor is complicatedly implemented on an SOI substrate by using a semiconductor process, it has a high production cost and has a large occupancy volume due to the occupied area of the SOI substrate even if it is manufactured in a minimum length unit using a semiconductor process, Since it uses SOI substrate, it has a limit to be used flexibly and has a possibility of explosion of hydrogen due to electric discharge because it has to use electricity.

Korean Patent Publication No. 10-2012-0088409 Korean Patent Publication No. 10-2006-0070749

SUMMARY OF THE INVENTION The present invention has been devised to solve the problems of the prior art, and it is an object of the present invention to provide a method of manufacturing a semiconductor device which does not use a substrate and electricity, A hydrogen sensing sensor, a method of manufacturing a hydrogen sensing sensor and a hydrogen sensing material suitable for reducing the possibility of hydrogen explosion due to electric discharge because it does not use electricity. It has its purpose.

The hydrogen sensing sensor according to the present invention comprises a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, and a plurality of platinum group-based particles respectively disposed on the plurality of titanium- A hydrogen sensing pigment comprising an oxide; And silicon mixed with the hydrogen sensing pigment, wherein the hydrogen sensing pigment and the silicon are mixed in a range of 3 g: 50 to 100 g.

The individual titanium based support particles may comprise titanium dioxide (TiO2).

The individual tungstate-based support particles may comprise tungstic acid (H 2 WO 4 ).

The individual platinum group oxides may comprise palladium (Pd).

The hydrogen sensing pigment may not return to the ivory color even when it is not in contact with the hydrogen in the air after it changes from ivory color to air,

The silicone may have a viscosity of 30,000 to 40,000 (cP).

The method for producing a hydrogen sensing sensor according to the present invention comprises mixing a first deionized water, a titanium based support powder and a tungstic acid based support powder to form a support solution, mixing a second deionized water, a hydrochloric acid and a platinum group chloride powder, Forming a hydrogen-sensing pigment by using the support solution and the deposition solution, and coating the hydrogen-sensing pigment with silicon, wherein the hydrogen-sensing pigment comprises a plurality of titanium-based support particles A plurality of tungsten-based support particles, and a plurality of the titanium-based support particles and the plurality of tungstic acid-based support particles, the hydrogen-sensing pigment and the silicon being formed by coating each of the tungsten- 100 g. ≪ tb > < TABLE >

The support solution is formed by preparing the first deionized water, preparing the titanium-based support powder, preparing the tungstic acid-based support powder, and adding the titanium-based support powder to 100 parts by weight of the first deionized water. 5 to 30 parts by weight of the powder and 1 to 10 parts by weight of the tungstic acid based support powder were mixed and the mixture of the first deionized water, the titanium based support powder and the tungstic acid based support powder was stirred at about 70 캜 for 1 hour As shown in FIG.

The deposition solution is formed by preparing the second deionized water, preparing the hydrochloric acid, preparing the platinum group chloride powder, and adding 10 to 50 parts by weight of the hydrochloric acid to 100 parts by weight of the second deionized water, 0.5 to 3 parts by weight of the platinum group chloride powder and mixing the second deionized water with the hydrochloric acid and the platinum group chloride powder at room temperature for 1 hour.

The formation of the hydrogen-sensing pigment was carried out by gradually adding the deposition solution to the support solution at about 70 DEG C, stirring the first solution of the support solution and the deposition solution for 1 hour Sodium hydroxide is added to the first mixed solution to accelerate the reaction of the deposition solution with respect to the support solution in the first mixed solution to maintain the pH of the first mixed solution in the range of 10 to 11, Hydrochloric acid is added to the second mixed solution to terminate the reaction of the deposition solution with respect to the support solution in the second mixed solution when the stirring time reaches the one hour, To a pH of about 8 to form a suspension, filtering the suspension through a filter paper to obtain a reserve hydrogen sensing pigment, The claim can include 3 to be washed with deionized water, and dried to form the wash the pre-detected hydrogen Pigment from about 100 ℃.

Coating the hydrogen sensing pigments with silicon may comprise preparing the hydrogen sensing pigments, preparing the silicon, and blending the hydrogen sensing pigments in the silicon.

The hydrogen sensing material according to the present invention includes a hydrogen sensing line; And a reference color line adjacent to the hydrogen sensing line, wherein the hydrogen sensing line is formed by mixing hydrogen sensing pigment and silicon in a range of 3 g: 50 to 100 g, Wherein the hydrogen sensing pigment comprises a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, and a plurality of titanium-based support particles and a plurality of tungsten acid-based support particles Wherein the reference color line includes a plurality of platinum group oxides that are respectively disposed on the support particles and before the hydrogen contact line of the hydrogen sensing line is contacted with hydrogen, The same color as that of the color is applied on the above-mentioned goods in a straight line, And is a kinematic film line.

Wherein the hydrogen sensing line absorbs the hydrogen through the silicon upon contact with the hydrogen in the air, and after the contact between the hydrogen sensing pigment and the hydrogen, converts the color converted through the color conversion of the hydrogen sensing pigment into the silicon. It can be displayed outside.

The hydrogen sensing line may have irreversible characteristics that do not return to the original color when the hydrogen is not in contact with the hydrogen in the air after the same color as the reference color line in contact with the hydrogen in the air.

The article may comprise a tape, glove, band or fitting cover.

The present invention relates to a process for producing a hydrogen-containing gas, which is painted on the surface of at least one of a transfer pipe, a reaction pipe and a discharge pipe located on the outer wall of the hydrogen reaction device or the hydrogen production device and around the hydrogen reaction device or the hydrogen production device, Hydrogen can be easily detected through the change of paint color during contact.

In order to detect hydrogen in the air, the present invention is applied in the form of paint on a sundial (= tape, glove, band, fitting cover, etc.) so that it does not depend on the shape of the goods and does not use electricity. The degree of freedom of use can be increased.

Since the present invention uses a sundial without any deformation of the structure of the product, the product is simply coated on the product in the form of a paint, so that the unit price required for sensing hydrogen is low and hydrogen is detected during use of the product, And can be flexibly used because it is implemented along the shape of the article.

The present invention is realized when paint is applied on a sundial so that the accumulation of electric charge does not occur on the coating line due to the sensing of hydrogen in the air even when electricity is not applied to the coating film line, .

1 and 2 are flowcharts illustrating a method of manufacturing a hydrogen sensing sensor according to the present invention.
FIG. 3 is a schematic view showing a container filled with the hydrogen sensing sensor manufactured by the method of manufacturing the hydrogen sensing sensor of FIGS. 1 and 2. FIG.
FIG. 4 is an image showing the color conversion of the hydrogen sensor before and after the hydrogen reaction in air of the hydrogen sensor of FIG. 3; FIG.
FIG. 5 is a graph showing the brightness (L value in a colorimeter) of the hydrogen sensor according to the contents of tungstic acid (H 2 WO 4 ) and palladium (Pd) before and after the reaction between hydrogen sensing sensor and hydrogen.
FIG. 6 is a schematic view showing a hydrogen sensing tape including a hydrogen sensing line and a reference color line using the hydrogen sensing sensor of FIG. 3. FIG.
FIG. 7 is a schematic diagram showing a hydrogen sensing glove including a hydrogen sensing line and a reference color line using the hydrogen sensing sensor of FIG. 3. FIG.
FIGS. 8 and 9 are schematic views showing a hydrogen sensing fitting cover including a hydrogen sensing line and a reference color line using the hydrogen sensing sensor of FIG. 3. FIG.

The following detailed description of the invention refers to the accompanying drawings, which illustrate, by way of illustration, specific embodiments in which the invention may be practiced. These embodiments are described in sufficient detail to enable those skilled in the art to practice the invention. It should be understood that the various embodiments of the present invention are different, but need not be mutually exclusive. For example, certain features, structures, and characteristics described herein may be implemented in other embodiments without departing from the spirit and scope of the invention in connection with one embodiment. It is also to be understood that the position or arrangement of the individual components within each disclosed embodiment may be varied without departing from the spirit and scope of the invention. The following detailed description is, therefore, not to be taken in a limiting sense, and the scope of the present invention is to be limited only by the appended claims, along with the full scope of equivalents to which such claims are entitled, if properly explained. In the drawings, like reference numerals refer to the same or similar functions throughout the several views, and length and area, thickness, and the like may be exaggerated for convenience.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings, so that those skilled in the art can easily carry out the present invention.

1 and 2 are flowcharts illustrating a method of manufacturing a hydrogen sensing sensor according to the present invention.

Referring to FIGS. 1 and 2, a method for manufacturing a hydrogen sensor (94 in FIG. 3) according to the present invention comprises: mixing a first deionized water, a titanium-based support powder and a tungstic acid-based support powder to form a support solution (S10). The support solution (S10) is prepared by preparing first deionized water, preparing a titanium-based support powder, adding 5 to 30 parts by weight of a titanium-based support powder to 100 parts by weight of the first deionized water, 1 to 10 parts by weight of a support powder, and mixing the mixture of the first deionized water, the titanium-based support powder and the tungstic acid-based support powder at about 70 ° C for 1 hour.

If the amount of the titanium based support powder is less than 5 parts by weight, since the titanium based support powder is dispersed in the first deionized water in a small amount, the number of the titanium based support particles (described below) The amount of sensor 94 can not be made in one attempt. If the amount of the titanium-based support powder is 30 parts by weight or more, the titanium-based support powder does not easily agitate in the first deionized water.

As shown in FIG. 5, when the tungstic acid-based support powder is not more than 1 part by weight, the tungstic acid-based support powder contains 2 to 5 parts by weight of the hydrogen sensing sensor 94 (L value measured in the color difference meter) of the hydrogen sensor 94, it does not contribute to the change of the visibility of the hydrogen sensor 94 under 1 part by weight.

5, when the tungsten support powder is not less than 10 parts by weight, the tungsten support powder may have a too low brightness of the hydrogen sensing sensor 94 after the hydrogen sensing sensor 94 reacts with hydrogen. It is difficult to control the color of the hydrogen sensing sensor 94. [0050]

After the support solution is formed, the deposition solution may be formed by mixing the second deionized water, hydrochloric acid and the platinum group chloride powder (S20). (S20), the second deionized water is prepared, hydrochloric acid is prepared, and a platinum group chloride powder is prepared. To 100 parts by weight of the second deionized water, 10 to 50 parts by weight of hydrochloric acid, Based chloride powder and 0.5 to 3 parts by weight of a chloride powder are mixed and the mixture of the second deionized water and the hydrochloric acid and the platinum group chloride powder is stirred at room temperature for 1 hour.

Here, the first deionized water and the second deionized water are deionized water of the same kind. If the amount of the hydrochloric acid is 10 parts by weight or less, the hydrochloric acid can not smoothly mix with the second deionized water and the platinum group chloride powder. If the amount of the hydrochloric acid is 50 parts by weight or more, the hydrochloric acid makes it difficult to adjust the pH required for the subsequent reaction and increases the acidity to increase the risk.

If the amount of the platinum group chloride powder is less than 0.5 part by weight, the platinum group chloride powder is dispersed in the second deionized water in a small amount. Therefore, the amount of the platinum group oxide (described below) It does not react sufficiently with the particles, so that the desired amount of the hydrogen sensor 94 can not be made in one attempt. If the amount of the platinum group chloride powder is 3 parts by weight or more, the platinum group chloride powder is highly dispersed in the second deionized water, thereby reducing the efficiency of formation of the hydrogen sensor 94 and increasing the acidity to increase the risk.

 After the deposition solution is formed, a hydrogen-sensing pigment may be formed using the support solution and the deposition solution (S70). 2, the support solution and the deposition solution are reacted (S30), and it is determined whether the reaction time of the support solution and the deposition solution is the same as the reference time (S40 ), Forming a suspension (S50), and collecting fine particles from the suspension (S60).

The step (S30) of reacting the support solution with the deposition solution may include slowly adding the deposition solution to the support solution at about 70 ° C by one drop. (S40) of confirming whether the reaction time of the support solution and the deposition solution is the same as the reference time, when the stirring time has not reached 1 hour, the first mixed solution of the support solution and the deposition solution is stirred for 1 hour Sodium hydroxide is added to the first mixed solution so as to accelerate the reaction of the deposition solution with respect to the support solution in the first mixed solution to maintain the pH of the first mixed solution in the range of 10 to 11, Lt; / RTI >

The suspension (S50) may be prepared by adding hydrochloric acid to the second mixed solution to terminate the reaction of the deposition solution with respect to the support solution in the second mixed solution when the stirring time reaches one hour, Lt; RTI ID = 0.0 > 8 < / RTI > (S60) of collecting fine particles from the suspension is performed by filtering the suspension through a filter paper to secure a spare hydrogen sensing pigment, washing the spare hydrogen sensing pigment with the third deionized water, washing the preliminary hydrogen sensing pigment Lt; RTI ID = 0.0 > 100 C. < / RTI >

The preliminary hydrogen sensing pigment may include a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, and a plurality of titanium-based support particles, a platinum group oxide surrounding the plurality of tungstic acid-based support particles, . The hydrogen sensing pigment may include a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, a plurality of platinum group-based oxides each of which surrounds a plurality of titanium-based support particles and a plurality of tungstic acid-based support particles . The titanium based support particles include titanium dioxide (TiO 2 ), the plurality of tungstic acid based support particles include tungstic acid (H 2 WO 4 ), and the platinum group oxide may include palladium (Pd) .

On the other hand, after the hydrogen sensing pigment is formed, the hydrogen sensing pigment may be coated with silicon (S80). The hydrogen sensing pigment is coated with silicon (S80). The hydrogen sensing pigment is prepared and gel state silicon (viscosity: 30,000 to 40,000 cP) is prepared. Hydrogen sensing pigment ≪ / RTI >

The hydrogen sensing pigment and silicon may be mixed in the range of 3 g: 50 to 100 g. Here, the mixture of hydrogen-sensing pigment and silicon does not include alcohols classified as dangerous substances and a nitrogen-containing compound.

FIG. 3 is a schematic view showing a container filled with the hydrogen sensing sensor manufactured by the method of manufacturing the hydrogen sensing sensor of FIGS. 1 and 2. FIG. 4 is a schematic view of the hydrogen sensing sensor of FIG. This is an image showing the color conversion of the sensor.

Referring to FIGS. 3 and 4, the hydrogen sensing sensor 94 filled in the container 96 includes hydrogen sensing pigment and silicon. The hydrogen sensing pigment includes a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, and a plurality of platinum group-based oxides respectively disposed on the plurality of titanium-based support particles and the plurality of tungstic acid-based support particles . The titanium-based support particles include titanium dioxide (TiO2). The plurality of tungsten-based support particles are tungstic acid (H 2 WO 4 ), and the platinum group oxide includes palladium (Pd).

The silicon is combined with a hydrogen sensing pigment. More specifically, the hydrogen sensing pigment and silicon are mixed in the range of 3 g: 50 to 100 g. Here, the mixture of hydrogen-sensing pigment and silicon does not include alcohol and toluene classified as hazardous materials. Therefore, the hydrogen sensor 94 is made of a safe material and is environmentally friendly.

Here, the silicon is in contact with hydrogen in the air to transfer hydrogen to the hydrogen sensing pigment, and the hydrogen sensing pigment reacts with hydrogen in the air from the ivory color 97 before or before the reaction with hydrogen in the air in FIG. (98) from the light gray (98) to the ivory color (97) even in the non-contact with hydrogen in the air after changing along the first direction (F1) Irreversible properties that do not go away. That is, the hydrogen sensor 94 has an ivory color 97 in the container 96 when the hydrogen sensor 94 does not react with hydrogen in the air or when it is not in contact.

Meanwhile, the hydrogen sensor 94 may be painted on the surface of at least one of a transfer pipe, a reaction pipe, and a discharge pipe located on the outer wall of the hydrogen reaction device or the hydrogen production device and around the hydrogen reaction device or the hydrogen production device. do.

FIG. 5 is a graph showing the brightness (L value in a colorimeter) of the hydrogen sensor according to the contents of tungstic acid (H 2 WO 4 ) and palladium (Pd) before and after the reaction between hydrogen sensing sensor and hydrogen. Here, the color difference meter is a standard colorimeter, and is a device that quantitatively indicates a color difference by measuring a comparison value with the standard color. Specifically, the colorimeter represents the brightness of an object as an L value.

The L value is interpreted as being closer to black when the L value is closer to 0 and closer to white when the L value is closer to 100. The L value is interpreted as being closer to white when the L value is applied to the hydrogen sensor (94 of FIG. 3) (Brightness and degree of darkness) of the color of the light source 94. [ In this case, the lightness of the hydrogen sensing sensor 94 is changed by changing the content of tungstic acid, titanium dioxide, palladium and silicon (tungstic acid) or palladium and fixing the remaining content, 5, respectively.

Referring to FIG. 5, the hydrogen sensing sensor 94 is formed by using 1 to 10 parts by weight of a tungstic acid-based support powder. Therefore, in order to simplify the description of the graph, the tungstic acid-based support powder will be briefly described as tungstic acid (H 2 WO 4 ). First, the change in the brightness (L value) of the hydrogen sensor 94 was confirmed as follows at 2, 5 and 10 parts by weight of tungstic acid.

Overall, in the tungstic acid 2, 5 and 10 parts by weight, the hydrogen sensor 94 shows a change in brightness from a dark color to a bright color as the content of tungstic acid increases before and after the hydrogen reaction. In addition, the hydrogen sensing sensor 94 has a brightness interval between before and after the hydrogen reaction in the tungstate 2, 5, and 10 parts by weight.

Specifically, the hydrogen sensing sensor 94 measures the lightness interval between before and after the hydrogen reaction in proportion to the remaining tungstic acid content in 5 parts by weight of tungstic acid 2, 5 and 10 parts by weight It has big. However, since 2, 5 and 10 parts by weight of tungstic acid makes the brightness gradient of the hydrogen sensing sensor 94 gentle before or after the hydrogen reaction, the manufacturing process of the hydrogen sensing sensor 94 is performed in a stable manufacturing environment It does.

Next, the hydrogen sensor 94 is formed using 0.5 to 3 parts by weight of a platinum group chloride powder. Here, in order to simplify the description of the graph, the platinum group chloride powder will be briefly described as palladium (Pd). The change in brightness (L value) of the hydrogen sensor 94 was confirmed as follows at palladium 1.5, 1.75 and 3 parts by weight.

Overall, in the palladium 1.5, 1.75 and 3 parts by weight, the hydrogen sensor 94 shows a change in brightness from a bright color to a dark color as the content of palladium increases after the hydrogen reaction and after the hydrogen reaction. In addition, the hydrogen sensing sensor 94 does not have a substantially constant brightness interval between hydrogen before and after the hydrogen reaction in palladium 1.5, 1.75, and 3 parts by weight.

Specifically, the hydrogen sensing sensor 94 has a very small brightness interval between before and after the hydrogen reaction in comparison with the remaining palladium content in 1.5 parts by weight of palladium 1.5, 1.75 and 3 parts by weight . In addition, since the palladium 1.5, 1.75 and 3 parts by weight make the brightness gradient of the hydrogen sensor 94 rush before or after the hydrogen reaction, the production process of the hydrogen sensor 94 is performed with tungstate 2, 5 and 10 parts by weight To be performed in an atmosphere of contrasting unstable manufacturing environment.

On the other hand, in order to test the visibility of the hydrogen sensing sensor 94 according to the brightness change before and after the hydrogen reaction based on the above-described phrase, the content of the tungstic acid is represented by a bright ivory color in the graph 2 parts by weight, and the content of palladium was selected to be 1.75 parts by weight, which shows a light brownishness.

That is, when the hydrogen sensing sensor 94 is manufactured by mixing 2 parts by weight of tungstic acid, titanium dioxide, palladium, silicon (tungstic acid) and 1.75 parts by weight of palladium into the remaining components, After the hydrogen reaction and the hydrogen reaction, the colors 97 and 98 shown in FIG. 4 were shown.

FIG. 6 is a schematic view showing a hydrogen sensing tape including a hydrogen sensing line and a reference color line using the hydrogen sensing sensor of FIG. 3. FIG. 7 is a schematic view showing a hydrogen sensing line and a reference color line ≪ / RTI > is a schematic diagram showing a hydrogen sensing glove containing hydrogen.

FIGS. 8 and 9 are schematic views showing a hydrogen sensing fitting cover including a hydrogen sensing line and a reference color line using the hydrogen sensing sensor of FIG. 3. FIG.

Referring to FIGS. 6 and 9, the hydrogen sensing tape (100 in FIG. 6) and the hydrogen sensing glove (110 in FIG. 7) are included in the hydrogen sensing article according to the present invention. The hydrogen sensing article includes a hydrogen sensing line 97a in each of the hydrogen sensing tape 100 and the hydrogen sensing glove 110 and a reference color line 98a adjacent to the hydrogen sensing line 97a. More specifically, the hydrogen sensing line 97a is located at the end of the hydrogen sensing tape 100 or the hydrogen sensing glove 110, and the reference color line 98a is positioned below the hydrogen sensing line 97a. do.

Here, the hydrogen sensing line 97a is formed on a sieve (= tape or glove) in the air by using a hydrogen sensing sensor 94 formed by mixing hydrogen sensing pigment and silicon in a range of 3 g: 50 to 100 g It is a film line which is film-processed in a straight line and with a certain thickness. The hydrogen sensing pigment includes a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, and a plurality of platinum group-based oxides respectively disposed on the plurality of titanium-based support particles and the plurality of tungstic acid-based support particles.

The hydrogen sensing line 97a absorbs hydrogen through contact with hydrogen in the air and displays the converted color through the silicon after exiting the contact between the hydrogen sensing pigment and the hydrogen sensing pigment. The color conversion of the hydrogen sensing pigment is performed in the same manner as in FIG. 4 depending on the presence or absence of hydrogen. The hydrogen sensing line 97a has the same color as the reference color line 98a when it comes into contact with hydrogen in the air and then has irreversible characteristics that do not return to the original color when not in contact with hydrogen in the air.

The reference color line 98a may be formed to have the same color as the discolored color of the hydrogen sensing line 97a during hydrogen contact in the air of the hydrogen sensing line 97a before and after the hydrogen contact of the hydrogen sensing line 97a, Which is a film line formed by coating a film of a predetermined thickness on a straight line. On the other hand, when the hydrogen sensing line 97a and the reference color line 98a are coated on the sundry goods (= band), a sundewater containing the hydrogen sensing line 97a and the reference color line 98a = Band) can be classified into a hydrogen sensing band (not shown in the figure) in the hydrogen sensing article.

In addition, when the hydrogen sensing line 97a and the reference color line 98a are coated on a sundial (= fitting cover), a sundial including the hydrogen sensing line 97a and the reference color line 98a The water (= fitting cover) can be classified as a hydrogen sensing fitting cover (128 in FIG. 8 or 149 in FIG. 9) in the hydrogen sensing article. The hydrogen sensing fitting cover 128 of FIG. 8 may wrap a cylindrical fitting 122 that receives the first pipe 124 and the second pipe 126 from two directions.

Here, the hydrogen sensing fitting cover 128 has elasticity on the cylindrical fittings 122 and includes hydrogen sensing lines 97a at both ends and a reference color line 98a at the central portion. The hydrogen sensing fitting cover 128 sufficiently covers an area between the first pipe 124 and the fitting 122 and an area between the second pipe 126 and the fitting 122. [ The hydrogen sensing fitting cover 128 exposes only the first pipe 124 and the second pipe 126 so that hydrogen leakage from the fitting 122 using the reference color line 98a and the hydrogen sensing line 97a Hydrogen can be detected.

The fittings 122, the first pipe 124, the second pipe 126, and the hydrogen sensing fitting cover 128 may constitute a pipe connection device 130. The hydrogen sensing fitting cover 149 shown in FIG. 9 can cover the 'T' shaped fittings 141 accommodating the first pipe 143, the second pipe 145 and the third pipe 147 from three directions have. Here, the hydrogen sensing fitting cover 149 has elasticity on the 'T' shaped fitting 141, and includes a hydrogen sensing line 97a at each end and a reference color line 98a at a central portion.

The hydrogen sensing fitting cover 149 is disposed between the first pipe 143 and the fitting 141 and between the second pipe 145 and the fitting 141 and the third pipe 147, And the area between the fittings 141 is sufficiently enclosed. Since the hydrogen sensing fitting cover 149 exposes only the first pipe 143, the second pipe 145 and the third pipe 147, the hydrogen sensing fitting cover 149 is fitted with the reference color line 98a and the hydrogen sensing line 97a, Hydrogen can be detected upon leakage of hydrogen from the flow 141.

The fittings 141, the first pipe 143, the second pipe 145, the third pipe 147 and the hydrogen sensing fitting cover 128 may constitute a pipe connection device 150. Alternatively, the hydrogen sensing fitting cover according to the modification of the present invention may wrap fittings accommodating pipes corresponding to individual directions from four or more directions. Here, the hydrogen sensing fitting cover according to the modification of the present invention may have a hydrogen sensing line at the end corresponding to the individual direction and a reference color line at the central portion.

94; Hydrogen sensor, 96; Vessel
97; Ivory color, 98; Light gray
97a; Hydrogen sensing line, 98a; Reference color line
100; Hydrogen sensing tape, 110; Hydrogen-sensing gloves

Claims (15)

A hydrogen sensing pigment comprising a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, and a plurality of platinum group-based oxides respectively disposed on the plurality of titanium-based support particles and the plurality of tungstic acid-based support particles; And
And silicon combined with the hydrogen sensing pigment,
Wherein the hydrogen sensing pigment and the silicon are mixed in a range of 3 g: 50 to 100 g.
The method according to claim 1,
Each of the titanium-based support particles comprises titanium dioxide (TiO2).
The method according to claim 1,
Wherein each of the tungsten acid based support particles contains tungstic acid (H 2 WO 4 ).
The method according to claim 1,
Wherein each of the platinum group oxides comprises palladium (Pd).
The method according to claim 1,
Wherein the hydrogen sensing pigment does not return to the ivory color even when it is not in contact with the hydrogen in the air after it changes from ivory color to air, Hydrogen sensor.
The method according to claim 1,
Wherein the silicon has a viscosity of 30,000 to 40,000 (cP).
The first deionized water, the titanium-based support powder and the tungstic acid-based support powder are mixed to form a support solution,
A second deionized water, a hydrochloric acid and a platinum group chloride powder are mixed to form a deposition solution,
Forming a hydrogen sensing pigment using the support solution and the deposition solution,
And coating the hydrogen sensing pigment with silicon,
Wherein the hydrogen sensing pigment comprises a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, and a plurality of the titanium-based support particles and the plurality of tungstic acid-based support particles,
Wherein the hydrogen sensing pigment and the silicon are mixed in a range of 3 g: 50 to 100 g.
8. The method of claim 7,
To form the support solution,
The first deionized water was prepared,
The titanium-based support powder is prepared,
The tungstic acid-based support powder was prepared,
5 to 30 parts by weight of the titanium-based support powder and 1 to 10 parts by weight of the tungstic acid-based support powder are mixed with 100 parts by weight of the first deionized water,
And a mixed solution of the first deionized water, the titanium-based support powder and the tungstic acid-based support powder is stirred at about 70 ° C for 1 hour.
8. The method of claim 7,
To form the deposition solution,
The second deionized water is prepared,
The hydrochloric acid was prepared,
The above-mentioned platinum group-based chloride powder was prepared,
10 to 50 parts by weight of hydrochloric acid and 0.5 to 3 parts by weight of the platinum group chloride powder are mixed with 100 parts by weight of the second deionized water,
The second deionized water, the hydrochloric acid and the platinum group chloride powder is stirred at room temperature for 1 hour.
8. The method of claim 7,
The formation of the hydrogen-
The deposition solution was slowly added to the support solution at about 70 캜,
The first solution of the support solution and the deposition solution is stirred for 1 hour and sodium hydroxide is added to the first solution to accelerate the reaction of the deposition solution to the support solution in the first mixture solution The pH of the first mixed solution is maintained in the range of 10 to 11 to form a second mixed solution,
When the stirring time reaches the one hour, hydrochloric acid is added to the second mixed solution to terminate the reaction of the deposition solution with respect to the support solution in the second mixed solution so that the pH of the second mixed solution is about 8 < / RTI > to form a suspension,
The suspension is filtered on a filter paper to obtain a reserve hydrogen-sensing pigment,
The preliminary hydrogen sensing pigment is washed with a third deionized water,
And drying the washed preliminary hydrogen sensing pigment at about 100 < 0 > C.
8. The method of claim 7,
The hydrogen-sensing pigment is coated with silicon,
The hydrogen sensing pigment is prepared,
The silicon was prepared,
And adding the hydrogen sensing pigment to the silicon.
Hydrogen sensing line; And
And a reference color line adjacent to the hydrogen sensing line,
The hydrogen sensing line is a coating film line formed by coating a film on a sintered product in a straight line and at a constant thickness in air using a hydrogen sensing sensor formed by mixing hydrogen sensing pigment and silicon in a range of 3 g:
Wherein the hydrogen sensing pigment includes a plurality of titanium-based support particles, a plurality of tungstic acid-based support particles, and a plurality of platinum group-based oxides respectively disposed on the plurality of titanium-based support particles and the plurality of tungstic acid- and,
The reference color line may have a color that is the same as the discolored color of the hydrogen sensing line at the time of hydrogen contact with air of the hydrogen sensing line before and after hydrogen contact of the hydrogen sensing line, Wherein the coated film line is a coating film line treated with a film.
13. The method of claim 12,
Wherein the hydrogen sensing line absorbs the hydrogen through the silicon upon contact with the hydrogen in the air, and after the contact between the hydrogen sensing pigment and the hydrogen, converts the color converted through the color conversion of the hydrogen sensing pigment into the silicon. Wherein the hydrogen-containing material is present on the outside of the hydrogen-sensing material.
13. The method of claim 12,
Wherein the hydrogen sensing line has an irreversible characteristic that when the hydrogen sensing line contacts the hydrogen in the air, the electrode exhibits the same color as the reference color line and then does not return to the original color when not in contact with the hydrogen in the air. Goods.
13. The method of claim 12,
Wherein the article comprises a tape, glove, band or fitting cover.
KR1020170071659A 2017-06-08 2017-06-08 Hydrogen-detecting sensor, method of forming the hydrogen-detecting sensor, and hydrogen-detecting miscellaneous goods KR101990120B1 (en)

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