JP2020024157A - Moisture absorbing and releasing amount measurement method and moisture absorbing and releasing amount measuring device - Google Patents

Abstract

To provide a moisture absorbing and releasing amount measurement method and a moisture absorbing and releasing amount measuring device capable of executing a more accurate measurement and evaluations for moisture absorbing properties and moisture releasing properties of a measurement sample.SOLUTION: A moisture absorbing and releasing amount measuring device 10 includes: a first chamber 11 capable of retaining the inside in a first atmosphere having a predetermined temperature and moisture; a second chamber 12 capable of retaining the inside in a second atmosphere in which at least one of temperature and moisture differs from that of the first atmosphere; movement means 13 for moving a moisture-absorbing sample 50 from the first chamber 11 to the second chamber 12; and mass measurement means 16 provided inside the second chamber 12.SELECTED DRAWING: Figure 1

Description

  The embodiment of the present invention relates to a method and apparatus for measuring the amount of moisture absorption / desorption in a hygroscopic sample.

  The hygroscopic sample absorbs or releases moisture according to a change in its external environment, and takes in or releases water vapor into the sample. For example, glass provided in a vehicle such as an automobile and separating the inside and the outside of the vehicle may be clouded due to moisture in the atmosphere depending on the usage environment. In order to prevent such fogging, there is known an antifogging glass in which an antifogging film having high moisture absorption performance is formed on a glass surface.

  By the way, in this anti-fog glass, the anti-fog performance was evaluated by measuring the change in the moisture absorption state when the atmosphere was changed in a chamber and a high-temperature and high-humidity environment, and further the timing of the occurrence of dew condensation and frost. (For example, see Patent Documents 1 and 2). Further, the inside of the walk-in chamber is set to a predetermined atmosphere, and a glove box provided with a Peltier element or the like capable of cooling a measurement sample is provided inside the walk-in chamber, and measurement is performed while changing the environment.

  However, according to these methods, since the atmosphere is basically changed in one chamber, there are limitations for that purpose, and in many cases, the initial environment setting is not sufficient. It is difficult to accurately measure the effects of changes.

  On the other hand, two chambers that can be set to a predetermined atmosphere are prepared, and the environment is changed by moving between the chambers. However, the sample was exposed to an external atmosphere, and a state change that could not be neglected in the evaluation of the moisture absorption or moisture release of the measurement sample might occur, so that accurate measurement was also difficult.

JP-A-2003-50219 JP 2010-190601 A

  Therefore, the present invention eliminates factors that affect the measurement result (based on the measurement environment, measurement method, etc.) as much as possible, and more accurately measure the moisture absorption characteristics or moisture release characteristics of the measurement sample based on environmental changes. It is an object of the present invention to provide a method for measuring the amount of moisture absorbed and released and an apparatus for measuring the amount of moisture absorbed and released, which can perform the evaluation.

  The method for measuring the amount of moisture absorption and desorption according to the present invention comprises: adapting a moisture-absorbent sample to a first atmosphere having a predetermined temperature and humidity; and applying the moisture-absorbent sample adapted to the first atmosphere to the first atmosphere. The method is characterized in that the sample is moved to a second atmosphere in which at least one of temperature and humidity is different from the atmosphere, and the mass of the hygroscopic sample is measured with time in the second atmosphere.

  The moisture absorption and desorption amount measurement device of the present invention includes a first chamber capable of holding the inside thereof in a first atmosphere having a predetermined temperature and humidity, and an interior having the first atmosphere having at least temperature and humidity. A second chamber, one of which can be held in a different second atmosphere, a moving means for moving the hygroscopic sample from the first chamber to the second chamber, and a moving means provided in the second chamber. Mass measuring means provided.

  ADVANTAGE OF THE INVENTION According to the moisture absorption / desorption amount measuring method and moisture absorption / desorption amount measuring apparatus of this invention, more accurate measurement and evaluation can be performed about the moisture absorption or moisture release of the measurement sample.

BRIEF DESCRIPTION OF THE DRAWINGS It is sectional drawing which showed schematic structure of the moisture absorption / desorption amount measuring apparatus which is one Embodiment of this invention. It is the graph which represented typically the mass change of the hygroscopic sample in the moisture absorption / desorption amount measuring method which is one Embodiment of this invention. It is sectional drawing which showed the schematic structure of the moisture absorption / desorption amount measuring apparatus which is another embodiment of this invention. It is sectional drawing which showed the schematic structure of the moisture absorption / desorption amount measuring apparatus which is another embodiment of this invention.

  Hereinafter, the method for measuring the amount of absorbed and released moisture and the apparatus for measuring the amount of absorbed and released moisture of the present invention will be described in detail with reference to embodiments.

[First Embodiment]
(Moisture absorption / desorption measurement device)
A moisture absorption / desorption measuring device according to an embodiment of the present invention will be described with reference to FIG. FIG. 1 is a cross-sectional view showing a schematic configuration of a moisture absorption / desorption amount measuring device. The moisture absorption / desorption amount measuring device 10 shown here includes a first chamber 11, a second chamber 12, and a first chamber 12. Moving means 13 for moving the hygroscopic sample 50 from the first chamber 11 to the second chamber 12.

  Further, the first chamber 11 and the second chamber 12 are usually connected by a passage 14. At least one openable and closable shutter 15 is provided inside the passage 14 so as to partition the first chamber 11 and the second chamber 12 from each other. Further, inside the second chamber 12, a mass measuring means 16 capable of measuring the mass of the hygroscopic sample 50 is provided.

  Hereinafter, each component of the moisture absorption and desorption amount measuring apparatus 10 of the present embodiment will be described.

  The first chamber 11 used in the present embodiment is a thermo-hygrostat that can maintain the inside of the chamber at a predetermined temperature and humidity, and has therein a hygroscopic sample 50 whose moisture absorption and desorption characteristics are to be measured. Any container that can be stably placed may be used.

  The first chamber 11 is formed of a material capable of forming a closed space without being affected by the external atmosphere and the internal atmosphere. Examples of such a material include metals, ceramics, glass, resins, and the like, and metals and ceramics are preferable. Examples of the metal include stainless steel, and examples of the resin include an acrylic resin and a vinyl chloride resin.

  An opening is formed in the first chamber 11 so that the hygroscopic sample 50 can be taken in and out. This opening is used when the hygroscopic sample 50 is moved from the first chamber 11 to the second chamber 12. This opening is connected to the opening of the second chamber through the passage 14, and is configured so that the hygroscopic sample 50 does not come into contact with the external atmosphere.

  The second chamber 12 used in the present embodiment is a thermo-hygrostat that can maintain the inside of the chamber at a predetermined temperature and humidity, and stores the mass of the hygroscopic sample 50 whose moisture absorption and desorption characteristics are to be measured. It is a place to measure.

  The second chamber 12 is formed of a material capable of forming a closed space without being affected by the external atmosphere and the internal atmosphere. Examples of such a material include metals, ceramics, glass, and resins, and metals and ceramics are preferable. Examples of the metal include stainless steel, and examples of the resin include an acrylic resin and a vinyl chloride resin.

  The second chamber 12 has an opening so that the hygroscopic sample 50 can be taken in and out. This opening is used when the hygroscopic sample 50 is moved from the first chamber 11 to the second chamber 12, as described above. This opening is connected to the opening of the first chamber through the passage 14, and is configured so that the hygroscopic sample 50 does not come into contact with the external atmosphere.

  Here, the predetermined temperature and humidity maintained in the second chamber 12 are maintained under conditions different from the predetermined temperature and humidity in the first chamber 11.

  The moving unit 13 used in the present embodiment is a unit that moves the hygroscopic sample 50 from the inside of the first chamber 11 to the inside of the second chamber 12. The moving means 13 may be any means that can stably and quickly move the hygroscopic sample 50, and examples thereof include a belt conveyor, a linear conveyor, and a roller conveyor.

  The passage 14 used in the present embodiment connects the first chamber 11 and the second chamber 12, and the inside thereof is a path for moving the hygroscopic sample 50. Therefore, the moving means 13 is usually provided inside the passage 14.

  Even when moving in the passage 14, the closed state can be formed so that the internal atmosphere of the passage 14 can be maintained at a predetermined temperature and humidity so that the hygroscopic sample 50 does not come into contact with the external atmosphere. Therefore, the same material as that of the first chamber 11 and the second chamber 12 can be used for the material of the passage 14.

  The passage 14 may have an opening that can be connected to an external atmosphere through which the hygroscopic sample 50 can be taken in and out. With such an opening, it is possible to prevent the inside of the first chamber 11 and the second chamber 12 from flowing directly with the external atmosphere, and it is possible to significantly suppress the fluctuation of the atmosphere in each chamber. Further, in order to maintain the internal atmosphere of the passage 14 as described above, a door that can be opened and closed is provided at this opening.

  The shutter 15 used in the present embodiment is an openable and closable member that is provided inside the passage 14 and partitions the first chamber 11 and the second chamber 12. At least one shutter 15 is provided.

  As shown in FIG. 1, a shutter 15 a and a shutter 15 b are provided in the opening of the first chamber 11 and the opening of the second chamber 12, respectively, so that the first chamber 11 and the second chamber 12 are provided. , Each space of the passage 14 can be independently partitioned, which is preferable.

  The shutters 15a and 15b are provided so as to be independently openable and closable, and perform opening and closing operations in accordance with the movement timing of the hygroscopic sample 50. Therefore, it is preferable that each of the moving means 13 and the shutters 15a and 15b has a control means capable of controlling each of the moving means 13 and the shutters 15a and 15b so as to operate in conjunction with the movement timing of the hygroscopic sample 50. With such a control means, the measurement operation can be performed automatically, so that efficient measurement can be performed.

  Further, the shutter 15 only needs to be able to hold the atmosphere in each chamber so as to perform the operation required for the measurement, and may not necessarily be able to be sealed. In addition, as shown in FIG. 1, since the moving means 13 is provided across each chamber and the passage, it may be difficult to seal even in this respect, but an elastic body or a member having flexibility is used. By doing so, it can be closed to the extent that the atmosphere is maintained.

  The moving means 13 is provided only in the passage 14, and the movement from the first chamber 11 to the moving means 13 and the movement from the moving means 13 to the second chamber 12 are performed using a robot arm or the like. It is easy to close the opening of the first chamber 11 and the opening of the second chamber 12 with the shutter 15, so that the hermetically sealed state can be formed more reliably.

  The mass measuring means 16 used in the present embodiment is a mass measuring device capable of measuring the mass of the hygroscopic sample 50 moved from the first chamber 11 to the second chamber 12 over time. The mass measuring device may be any device that can measure a change in mass over time, and examples thereof include an electronic balance, a load sensor, and a load cell.

  The electronic balance may be any known electronic balance, and examples thereof include an electronic balance of an electric resistance wire type, a tuning fork type, a capacitance type, an electromagnetic balance type, and the like. As the electronic balance, any of a type in which an object to be measured is placed on a weighing platform, a type in which an object to be measured is suspended from above, and the like can be used.

  The first chamber 11 and the second chamber 12 can independently maintain the atmosphere in the chamber, but at least one of them has a first temperature and humidity in which the temperature and humidity in the chamber can be adjusted to a predetermined range. It has adjusting means. The first chamber 11 and the second chamber 12 can have different internal atmosphere conditions by the first temperature / humidity adjusting means. By setting the internal atmosphere in each chamber to a predetermined one, it becomes possible to easily and efficiently measure the moisture absorption / release characteristics of the moisture absorbent sample 50 due to environmental changes.

At this time, the sizes of the first chamber 11 and the second chamber 12 are not particularly limited as long as they have the above-described functions, but for example, the volume is preferably 8,000 to 64,000 cm ³ . It is preferable that the volume be 8000 cm ³ or more, because fluctuation of the atmosphere in the chamber caused by the opening and closing operation of the shutter 15 when the hygroscopic sample 50 moves during measurement can be suppressed. Meanwhile, since it takes the result in too large time adjustment to a predetermined atmosphere, thereby enabling efficient measurement as 64,000Cm ³ below.

The volume inside the passage 14 is not particularly limited as long as the hygroscopic sample 50 can be moved stably, and its size is not particularly limited, but is preferably 1,600 to 1,900 cm ³ , and 1,100 to 1,100 cm ^3. , 600 cm ³ is more preferred. It is preferable that the volume of the passage 14 is made as small as possible compared to the first chamber 11 and the second chamber 12 because fluctuations in the atmosphere in the first chamber 11 and the second chamber 12 can be suppressed.

  In order to suppress this fluctuation, the ratio of the volume of the passage 14 to the volume of the first chamber 11 and the volume of the second chamber 12 is preferably 1/4 or less, more preferably 1/5 or less, and 1/6 or less. More preferred. In particular, if this relationship is satisfied in the second chamber 12, this effect can be almost ignored in the measurement result.

(Method of measuring moisture absorption and desorption)
Next, a method for measuring the amount of absorbed and released moisture in the present embodiment will be described. As a method for measuring the amount of absorbed and released moisture, a case where the amount of absorbed and released moisture is measured using the above-described apparatus 10 for measuring the amount of absorbed and released moisture will be described as an example.

  The method for measuring the amount of moisture absorption and desorption according to the present embodiment is as follows. The moisture absorption sample 50 is adapted to a first atmosphere having a predetermined temperature and humidity, and the moisture absorption sample adapted to the first atmosphere is converted to a first atmosphere. Is to move to a second atmosphere in which at least one of temperature and humidity is different, and measure the mass of the hygroscopic sample 50 with time in the second atmosphere.

  The hygroscopic sample 50 used here is not particularly limited as long as it is a target for measuring the hygroscopic characteristics. Generally, the moisture-absorbing sample 50 is a sample having a moisture-absorbing property for taking in water vapor in the atmosphere or a moisture-releasing property for releasing taken-in moisture (water vapor) into the atmosphere.

  The hygroscopic sample 50 includes, for example, glass, resin, fiber, concrete, wood, and the like, and is typically glass. Glass is used as a window glass of a building, a window glass of a train or an automobile, a door glass, and the like, and is often provided as a boundary between indoor and outdoor. Therefore, both surfaces of such glass may be exposed to completely different environmental atmospheres depending on the temperature and humidity inside and outside the room. In addition, especially in a train or a car, the outside atmosphere changes greatly due to the movement, and is often placed in a different environment atmosphere.

  Then, when exposed to such a change in the environmental atmosphere, when moisture in the atmosphere is rapidly cooled on the glass surface, dew condensation occurs, and water droplets adhere to the glass surface, and the glass may become cloudy. On the other hand, anti-fog glass is known as a glass that suppresses such fogging even by environmental changes and suppresses such fogging. The anti-fog glass has a functional film (anti-fog film) having a hygroscopic property formed on the surface of the glass. The anti-fog glass can absorb or release moisture due to changes in the external environment, and can suppress the fogging of the glass surface due to condensation.

  In the present embodiment, first, when measuring the amount of absorbed and released moisture, the hygroscopic sample 50 to be measured is adapted to the first atmosphere having a predetermined temperature and humidity. Here, “adapted to the atmosphere” means a state in which the hygroscopic sample has reached an equilibrium state without mass fluctuation due to moisture absorption and moisture release.

  In order to adapt the moisture-absorbing sample 50 to the first atmosphere, the moisture-absorbing sample 50 may be placed in the first chamber 11 holding the interior of the sample in the first atmosphere for a predetermined time. . Here, the predetermined time is preferably 15 minutes or more, more preferably 30 minutes or more, and even more preferably 60 minutes or more.

  Alternatively, a mass measuring unit may be provided in the first chamber 11 to determine whether or not the moisture-absorbent sample 50 has been adapted to the condition while confirming the change in the mass. That is, when there is no change in the mass and the state of equilibrium is reached, it can be determined that the user is familiar.

  In order to introduce the hygroscopic sample 50 into the first chamber 11, the opening through which the hygroscopic sample 50 can be put in and out may be provided in the passage 14 as described above. At this time, the hygroscopic sample 50 may be moved into the first chamber 11 by placing the hygroscopic sample 50 on the moving means 13 in the passage 14 and then operating the moving means 13.

  In the first chamber 11, an opening for introducing the hygroscopic sample 50 may be provided separately from the opening connected to the passage 14, and in that case, the first chamber 11 may be introduced. Since the internal and external atmospheres can be directly circulated, the atmosphere in the first chamber 11 may fluctuate greatly, which is not preferable.

  Next, the hygroscopic sample 50 adapted to the first atmosphere is moved to a second atmosphere different in at least one of temperature and humidity from the first atmosphere.

  In this movement, the moving means 13 may move the hygroscopic sample 50 from the first chamber 11 to the second chamber 12. At this time, the first chamber 11 and the second chamber 12 are spatially partitioned by shutters 15 (shutters 15a and 15b), respectively, so that the internal atmosphere can be maintained.

  In the movement, the shutter 15a provided in the opening of the first chamber 11 is opened, and at the same time, the hygroscopic sample 50 is moved from the inside of the first chamber 11 into the passage 14 by the moving means 13. After moving the hygroscopic sample 50 into the passage 14, the shutter 15a is closed.

  Next, the shutter 15b provided at the opening of the second chamber 12 is opened, and at the same time, the hygroscopic sample 50 is moved from the inside of the passage 14 into the second chamber 12 by the moving means 13. After moving the hygroscopic sample 50 into the second chamber 12, the shutter 15b is closed.

  By moving in this manner, fluctuations in the respective atmospheres in the first chamber 11 and the second chamber 12 can be suppressed, and the amount of absorbed and released moisture can be measured. By suppressing the fluctuation in this way, a predetermined atmosphere can be maintained, and the amount of moisture absorption and desorption due to the fluctuation of the environment can be measured accurately.

  At this time, by making the ratio of the volume of the passage 14 to the volume of the first chamber 11 and the volume of the second chamber 12 sufficiently small, the above-described fluctuation can be more easily suppressed. The ratio is, for example, preferably 1/4 or less, more preferably 1/5 or less, and still more preferably 1/6 or less, as described above.

  The atmosphere inside the passage 14 does not need to be particularly controlled. In this case, when the shutter 15a is opened, the atmosphere inside the first chamber 11 becomes the first atmosphere, and when the shutter 15b is opened, the atmosphere inside the second chamber 12 is opened. Of the second atmosphere.

  At this time, the internal atmosphere in the passage 14 may be managed so as to be a third atmosphere having a predetermined temperature and humidity. When the atmosphere is managed as the third atmosphere, a second temperature / humidity adjusting means for adjusting the atmosphere in the passage 14 is provided.

  The third atmosphere is an atmosphere to which the hygroscopic sample 50 is exposed just before moving to the second chamber 12, and is the same as the first atmosphere so as to keep the hygroscopic sample 50 dry or wet. The conditions of the degree are preferable, and the same conditions are more preferable. By doing so, the fluctuation state of the hygroscopic sample 50 in an environmental change from the first atmosphere to the second atmosphere can be measured quickly and accurately.

  Then, the mass of the hygroscopic sample 50 moved into the second chamber is measured over time by the mass measuring means 16 in the second atmosphere.

  At this time, the mass of the hygroscopic sample 50 fluctuates roughly into two types, that is, the case where the mass increases due to moisture absorption and the case where the mass decreases as the moisture is released. Hereinafter, these cases will be described separately.

  First, when moisture is absorbed, a case where the first atmosphere is set to low temperature and low humidity and the second atmosphere is set to high temperature and high humidity can be exemplified. The terms low temperature-low humidity and high temperature-high humidity are relative expressions (the same applies hereinafter).

  In this case, a change in mass as shown in FIG. 2 can be exemplified. FIG. 2 is a conceptual diagram in which the hygroscopic sample 50 is moved into the second chamber 12 and the time from the start of mass measurement is plotted on the horizontal axis, and the change in mass of the hygroscopic sample 50 is plotted on the vertical axis. It is a graph. That is, it is a graph showing a change in state (mass) from when the hygroscopic sample 50 is exposed to the second atmosphere and measurement is started by the mass measuring means 16.

  As shown in FIG. 2, the hygroscopic sample 50 is adapted to the first atmosphere, and at the moment of moving to the second atmosphere, the air around the hygroscopic sample 50 is instantaneously cooled, The water vapor inside adheres to the surface of the hygroscopic sample 50. The attached moisture is absorbed into the inside by the hygroscopic property of the hygroscopic sample 50. At this time, the change on the surface is not confirmed visually or the like, but by measuring the mass and observing the change, the mass increases in accordance with the amount of absorbed water, and the mass of the water-absorbing sample 50 increases. It is becoming.

  If the moisture absorption characteristics of the moisture absorbing sample 50 exceed the saturated water absorption, water droplets and the like are generated on the surface of the moisture absorbing sample 50 (dew condensation occurs). In FIG. 2, the level of the saturated water absorption is indicated by a broken line. That is, the intersection of the dashed line and the solid line representing the mass variation of the hygroscopic sample 50 indicates the moment of dew condensation. As the mass becomes heavier beyond the dashed line, the dew condensation occurs on the surface of the hygroscopic sample 50. Indicates that the amount of water drops has increased.

  In addition, when the first dew point in the first atmosphere at the temperature T1 and the humidity H1 is D1, and the second dew point temperature D2 in the second atmosphere at the temperature T2 and the humidity H2 is D2, FIG. Under the described conditions, the temperature T1 in the first atmosphere is preferably lower than the second dew point temperature D2 (T1 <D2). That is, in this case, the temperature of the hygroscopic sample 50 is the temperature T1 of the first atmosphere because it is adapted to the first atmosphere, and this is exposed to the second atmosphere. At this time, if the temperature T1 of the first atmosphere is lower than the second dew point temperature D2, the second atmosphere is cooled around the hygroscopic sample 50, and the hygroscopic sample 50 easily absorbs moisture. Is generated, a mass that increases in accordance with the amount of moisture absorption is measured. Further, the temperature T1 is preferably lower than the second dew point temperature D2 by 2 ° C. or more, and more preferably lower by 5 ° C. or more.

  In other conditions including temperature and humidity, for example, the temperature T1 of the first atmosphere is lower than the second dew point temperature (D2) ° C., the humidity H1 is 0 to 90% RH, and the temperature T2 of the second atmosphere is Is 0 to 40 ° C, humidity H2 is 30 to 90% RH, temperature T1 is less than [(D2) -2] ° C, humidity H1 is 30 to 90%, temperature T2 is 0 to 20 ° C, and humidity H2 is 50 to 90% RH is preferable, temperature T1 is less than [(D2) -5] ° C, humidity H1 is 50 to 90%, temperature T2 is 0 to 10 ° C, and humidity H2 is 70 to 90% RH.

  Further, in the case where moisture is released contrary to FIG. 2, the case where the first atmosphere is set to low temperature and high humidity and the second atmosphere is set to high temperature and low humidity can be exemplified.

  In this case, the hygroscopic sample 50 is adapted to the first atmosphere, and at the moment of moving to the second atmosphere, the air around the hygroscopic sample 50 is instantaneously cooled, and the water vapor in the air absorbs moisture. Adheres to the surface of the neutral sample 50. However, since the first atmosphere was in a high-humidity condition, the moisture-absorbing sample 50 absorbed moisture to some extent, and the second atmosphere was in a low-humidity condition, so that moisture was released from the moisture-absorbing sample 50 to the second atmosphere. Is dominant. At this time, by measuring the mass and observing the fluctuation, it is understood that the mass decreases in accordance with the amount of released water, and the mass of the water-absorbing sample 50 decreases.

  Similarly to the above, when expressed under the conditions of the first atmosphere and the second atmosphere, for example, the temperature T1 of the first atmosphere exceeds the second dew point temperature (D2) ° C., the humidity H1 is 30 to 90% RH, The temperature T2 of the atmosphere 2 is 0 to 40 ° C., the humidity H2 is 0 to 90% RH, the temperature T1 is higher than ((D2) +2] ° C., the humidity H1 is 50 to 90%, and the temperature T2 is 10 to 40%. ° C, humidity H2 is preferably 0 to 70% RH, temperature T1 is more than [(D2) +5] ° C, humidity H1 is 70 to 90%, temperature T2 is 20 to 40 ° C, and humidity H2 is 0 to 50% RH. More preferred.

  In addition, examples of the case where moisture is released include a case where the first atmosphere is set to high temperature and high humidity and the second atmosphere is set to low temperature and low humidity.

  In this case, the moisture-absorbing sample 50 is adapted to the first atmosphere, and at the moment of moving to the second atmosphere, the air around the moisture-absorbing sample 50 is instantaneously warmed, Since the transfer is to the condition, moisture is released from the hygroscopic sample 50 to the second atmosphere. At this time, by measuring the mass and observing the fluctuation, it is understood that the mass decreases in accordance with the amount of released water, and the mass of the water-absorbing sample 50 decreases.

  Similarly to the above, when expressed under the conditions of the first atmosphere and the second atmosphere, for example, the temperature T1 of the first atmosphere exceeds the second dew point temperature (D2) ° C., the humidity H1 is 30 to 90% RH, The atmosphere T2 has a temperature T2 of −10 to 30 ° C., a humidity H2 of 0 to 90% RH, a temperature T1 of more than ((D2) +2] ° C., a humidity H1 of 50 to 90%, and a temperature T2 of −5. -30 ° C, humidity H2 is preferably 0-70% RH, temperature T1 is more than ((D2) +5] ° C, humidity H1 is 70-90%, temperature T2 is 0-30 ° C, and humidity H2 is 0-50%. RH is more preferred.

  As described above, the moisture absorption and desorption amount measuring device and the moisture absorption and desorption amount measuring method in the first embodiment have been described. As a modified example, the moisture absorption and desorption amount measuring device 20 shown in FIG. The moisture absorption / desorption amount measuring apparatus 20 further includes a third chamber 21, and the mass measurement means is a hanging type mass measurement means 22 which suspends the hygroscopic sample 50 to be measured from above. It is different from the humidity measuring device 10. Other than that, it is the same as the moisture absorption / desorption amount measuring apparatus 10, and the same reference numerals are given to the reference numerals.

  The third chamber 21 is a container for accommodating the hygroscopic sample 50 that has been adjusted to the first atmosphere in the first chamber 11, as shown in FIG. The third chamber 21 is moved from the first chamber 11 to the second chamber 12 while holding the hygroscopic sample 50. At this time, the inside of the third chamber 21 is maintained at the same or the same atmosphere condition as the first atmosphere. Then, in the second chamber 12, the third chamber 21 is opened, and the hygroscopic sample 50 is exposed to the second atmosphere.

  In the case where the mass measurement is performed by the hanging-type mass measuring unit 22, for example, a metal member such as a clip is fixed to four sides of the hygroscopic sample 50, and this is provided at a position corresponding to the mass measuring unit 22. The mass measurement can be performed by attracting the magnet.

  In FIG. 3, as a supplement, a lifter 23 that lifts the hygroscopic sample 50 together with the third chamber 21 and allows the hygroscopic sample 50 to approach the mass measurement unit 22 is provided at the bottom in the second chamber 12. Is shown. This lifter 23 can move a vertically extending pin up and down, raise the hygroscopic sample 50 or the third chamber 21 at the tip of the pin, bring the hygroscopic sample 50 close to the magnet of the mass measuring means 22, It is possible to adsorb.

  In this case, the sample can be moved into the second chamber 12 while reliably maintaining the atmosphere in contact with the hygroscopic sample 50. In this case, the passage 14 does not need to be maintained at the predetermined temperature and humidity.

[Second embodiment]
Next, an apparatus for measuring the amount of moisture absorbed and released according to another embodiment of the present invention will be described with reference to FIG. FIG. 4 is a cross-sectional view showing a schematic configuration of the moisture absorption / desorption amount measuring device. The moisture absorption / desorption amount measuring device 30 shown here is similar to the moisture absorption / desorption amount measuring device 10 in the first chamber 11. , A second chamber 12, a moving unit 13, a passage 14, a shutter 15, and a mass measuring unit 16, and further, condensation and condensation on the surface of the hygroscopic sample 50 in the second chamber 12. It has dew condensation and frost detection means 31 that can detect the occurrence of frost. That is, the moisture absorption and desorption amount measuring device 30 has the same configuration as the moisture absorption and desorption amount measuring device 10 except that the device has a dew condensation and frost detection means 31. Therefore, in the following description, description of the same configuration will be omitted, and only different points will be described.

  In the present embodiment, since the apparatus has the dew condensation and frost detection means 31, in addition to the measurement of the amount of moisture absorption and desorption, the state of occurrence of dew condensation and frost can be evaluated, and the variation of the hygroscopic sample 50 due to environmental changes is examined in more detail. be able to. That is, when the hygroscopic sample 50 is the above-described anti-fog glass, the limit of the anti-fog performance can be measured.

  Here, the dew condensation and frost detection means 31 can detect whether dew condensation or frost has occurred on the surface of the hygroscopic sample 50 in the second chamber 12 as described above. The dew / frost detecting means 31 is not particularly limited as long as it can detect the occurrence of dew / frost on the surface of the hygroscopic sample 50. The occurrence of the condensation and frost is detected, for example, by detecting a change in the surface on an image by an imaging unit such as a camera, detecting an electrical change on the surface by an energized condensation sensor, or reacting by the presence of moisture. A substance can be used to detect or detect chemical changes.

  FIG. 4 illustrates a case where an image pickup unit such as a camera is provided as the dew / frost detection unit 31. The dew condensation and frost detection means 31 can photograph and observe the surface of the hygroscopic sample 50 placed on the mass measuring means 16. The photographed image is displayed on an external monitor so that the measurer can confirm the occurrence of dew condensation and frost.

  Further, the occurrence of dew condensation and frost may be detected by image analysis of the captured image. In this case, it is preferable to automatically detect the occurrence of dew condensation and frost efficiently and accurately on the computer.

  Also in the present embodiment, it is preferable to carry out under the same conditions as in the first embodiment. However, in the present embodiment, since dew condensation and frost can be detected, it is possible to sufficiently examine the moisture absorption characteristics of the hygroscopic sample 50 under conditions that reliably generate dew condensation and frost.

  Hereinafter, the present invention will be further described with reference to examples, but the present invention is not limited to these examples.

(Reference Example 1: Preparation of hygroscopic sample for evaluation)
A 0.76 mm polyvinyl butyral film is sandwiched and laminated between 2 mm glass and 2 mm glass, and an epoxy resin-based anti-fog coat consisting of a base layer and an upper layer is provided on one surface (inside the car) by a wet coating method, Windshield glass for automobile was obtained. From the windshield glass having the anti-fog coat, a square glass of 100 mm × 100 mm × 4.76 mm was cut out to prepare a hygroscopic sample 1 for evaluation. The thickness of the antifogging coat was 14 μm.

(Example 1)
The present embodiment is an example relating to conditions (environmental change from low-temperature to low-humidity to high-temperature to high-humidity) that cause moisture absorption, dew condensation, and frost formation. In the present embodiment, as a moisture absorption / desorption amount measuring device, the moisture absorption / desorption amount measuring device 30 shown in FIG. 4 has a basic configuration, and the mass measuring means 16 is changed to the mass measuring means 22 shown in FIG. (A lifter 23 was also used).
About the obtained hygroscopic sample 1, in order to observe the cloudiness state of the surface treated with the anti-fog coat, a black colored aluminum plate 3.0 mm was spread on 4.0 mm styrene foam, and the aluminum plate was placed on the aluminum plate. A non-freezing gel was applied thinly, and further overlaid thereon, with the anti-fog coating surface of the vapor-absorbing sample facing upward. Furthermore, a metal clip was fixed to four sides of the glass sample.

  Aluminum and gel are provided to increase the thermal conductivity and heat capacity and keep the temperature of the glass as constant as possible. In addition, since the styrene foam on the lowermost surface has a high heat insulating property and a small heat capacity, when the environmental temperature is changed, the styrene surface temperature has a high ability to follow the environmental temperature, and the dew condensation is small so as not to give an error to the weight measurement. That's why. The four metal clips are provided so as to be sucked and suspended by a magnet using a lower hanging measurement type electronic balance.

  The hygroscopic sample 1 thus obtained is placed in the center of the first chamber 11, and then the temperature T1 in the first chamber 11 is set to 0 ° C., and the relative humidity H1 is set to 70% RH. The hygroscopic sample 1 was soaked in the environment for 4 hours.

  In the second chamber 12, the temperature T2 was set at 10 ° C. and the relative humidity H2 was set at 70% RH (the dew point at 4.degree. C. and 70% RH was 4.78.degree. This is the condition under which moisture absorption / condensation occurs in the hygroscopic sample).

The shutter 15a on the first chamber 11 side was opened to connect the passage 14 with the first chamber 11, and the environmental atmosphere in the passage 14 was set to the environmental atmosphere of the first chamber 11. This prevented problems such as moisture absorption and dew condensation occurring while the hygroscopic sample 1 was moving in the passage 14.
The shutter 15a was closed, then the shutter 15b on the second chamber 12 side was opened, and the hygroscopic sample 1 was moved into the second chamber 12 by a belt conveyor.

  The lifter is lifted from the lower part of the hygroscopic sample 1 stopped at the center of the second chamber, the hygroscopic sample 1 is lifted, adsorbed on the measuring rod of the hanging electronic balance 16, and the mass measurement is started while being hung. Then, a change in mass over time was measured. The adsorption of the light weight rod to the hanging electronic balance was performed by fixing steel clips on the four sides of the upper surface of the hygroscopic sample 1 and providing magnets corresponding to the positions of the steel clips.

  Simultaneously with the above measurement, the dew / frost state on the surface of the moisture-absorbing sample 1 is observed with a video camera provided inside the second chamber 12, and the surface of the moisture-absorbing sample 1 becomes white due to the occurrence of condensation and frost. The time was recorded.

In this example, after 330 seconds condensation was observed from the start of measurement, the mass increase 15mg next at that time, divided by the sample area 100 mm × 100 mm, with moisture absorption amount per unit area 1.5 g / ^{m 2} there were.

  Incidentally, a test was performed under the same conditions as in Example 1 except that T1 was set to −2 ° C., with the laminated glass 1 not subjected to the anti-fog coating treatment of the hygroscopic sample 1 as a sample. That is, the atmosphere in the first chamber 11 has T1 of −2 ° C. and H1 of 70% RH, and the atmosphere in the second chamber 12 has T2 of 10 ° C., H2 of 70% RH and the second dew point. The temperature is 4.78 ° C.

In this test, after transferring the laminated glass 1 to the second chamber 12, dew condensation and frost were observed 5 seconds later, and the mass increase due to moisture absorption was less than 0.1 g / m ² per unit area.

(Example 2)
The present embodiment is an example relating to conditions for causing moisture release (environmental change from low temperature-high humidity to high temperature-low humidity).
The hygroscopic sample 1 was placed in the center of the first chamber 11 in the same manner as in Example 1, and then the temperature T1 in the first chamber 11 was set at 10 ° C., and the relative humidity H1 was set at 90% RH. Then, the hygroscopic sample 1 was soaked in the environment for 4 hours.

  In the second chamber 12, the temperature T2 was set at 35 ° C. and the relative humidity H2 was set at 10% RH (the dew point temperature in this atmosphere was −1.1 ° C., and T1 was 10 ° C. and the dew point temperature −1.1). If the initial equilibrium water absorption of the hygroscopic sample 1 is sufficiently high because the temperature is higher than ℃, a decrease in weight is observed by dehumidifying and drying.)

By the same operation as in Example 1, the hygroscopic sample 1 was moved from the first chamber 11 to the second chamber 12, and suspended mass measurement was started with an electronic balance, and the change in mass over time was measured. It was measured.
Here, the change in mass was continuously measured for 10 minutes, and the mass decrease at that time was 2.5 g / m ² per unit area, which was the amount of moisture released for dehumidification and drying.

The saturated water absorption capacity of the hygroscopic sample 1 was 5 g / m ² , and it was found from the above results that approximately 50% of the anti-fogging property could be recovered in 10 minutes.

(Example 3)
The present embodiment is an example relating to conditions for causing moisture release (environmental change from high temperature / high humidity to low temperature / low humidity).
The hygroscopic sample 1 was placed in the center of the first chamber 11 in the same manner as in Example 1, and then the temperature T1 in the first chamber 11 was set at 20 ° C., and the relative humidity H1 was set at 90% RH. Then, the hygroscopic sample 1 was soaked in the environment for 4 hours.

  In the second chamber 12, the temperature T2 was set at 10 ° C. and the relative humidity H2 was set at 50% RH (the dew point in this atmosphere was 0.05 ° C., and T1 was 20 ° C. and the dew point temperature was 0.05 ° C.). Therefore, if the initial equilibrium water supply amount of the hygroscopic sample 1 is sufficiently high, the mass loss is observed by dehumidifying and drying).

By the same operation as in Example 1, the hygroscopic sample 1 was moved from the first chamber 11 to the second chamber 12, and suspended mass measurement was started using an electronic balance, and the change in mass over time was measured. It was measured.
Here, the mass change was continuously measured for 10 minutes, and the mass decrease at that time was 3.8 g / m ² per unit area, which was the amount of moisture released for dehumidification and drying.

The saturated water absorption capacity of the hygroscopic sample 1 was 5 g / m ² , and it was found from the above results that approximately 76% of the anti-fogging property could be recovered in 10 minutes.

(Comparative Example 1)
As a conventional test method, a walk-in chamber (constant temperature / humidity chamber) (CH111P manufactured by ETAC) was prepared, and the atmosphere in the chamber was set at a temperature T2 of 10 ° C. and a relative humidity H2 of 70%. A sample provided with styrofoam and an aluminum plate on a 100 mm × 100 mm glass sample (hygroscopic sample 1) on which the antifogging coat obtained in Reference Example 1 was formed as in Example 1 was held in the chamber for 4 hours. Placed in equilibrium.

  A glove box was set in the chamber, a Peltier device cooling plate was prepared therein, and the temperature was cooled to 0 ° C. as T1. The size of the cooling plate used here is 150 × 150 cm.

  In the chamber, a moisture-proof film was stuck on the surface of the hygroscopic sample 1, placed on a Peltier element cooling plate in a glove box, and left to cool for 1 hour.

  The electronic balance was brought into the chamber, the hygroscopic sample 1 cooled by the Peltier cooling plate was taken out, and after removing the moisture-proof film on the surface, the mass increase was measured with the electronic balance, and at the same time, the dew condensation occurrence time was recorded by visual observation. .

  Although the mass change and the dew condensation time could be measured, it was difficult to evaluate because the initial equilibrium water absorption of the glass was different. That is, the equilibrium environment relating to the water absorption of the glass is such that the temperature T2 is 10 ° C., the relative humidity H2 is 70% RH, the moisture absorption film in that state is fixed by attaching a moisture-proof film to the surface, and then T1 is reduced to 0 by the Peltier element. Therefore, the state of the hygroscopic sample under the initial conditions of the temperature T1 of 0 ° C. and H2 of 70% RH cannot be accurately reflected.

(Comparative Example 2)
As another conventional test method, a test was performed in the same procedure as in Comparative Example 1 except that the humidity was changed as follows.
Equilibrium environment: temperature T1 at 0 ° C., relative humidity H1 at 20% RH
Test environment: temperature T2 at 10 ° C., relative humidity H2 at 70% RH
Also in this example, the initial equilibrium water absorption of the glass was different and the evaluation was difficult, and the test in which the humidity was changed could not be performed well.

(Comparative Example 3)
As a manual transfer test, two chambers were prepared. In the first chamber, the temperature T1 was set to −10 ° C., and the relative humidity R1 was set to 50%. The sample provided with the aluminum plate was placed in an equilibrium state for 4 hours. In the second chamber, a ceiling-mounted electronic balance was set, the temperature T2 was set to 0 ° C., and the relative humidity H2 was set to 90% RH. However, in this example, no member for maintaining the atmosphere such as a passage is provided between the first chamber and the second chamber, and the temperature and humidity are in the test chamber.

  Open the front door of the first chamber, take out the hygroscopic sample 1 by hand, open the front door of the second chamber, hang the hygroscopic sample 1 on an electronic balance, measure the mass change over time, and visually observe The occurrence time of dew condensation and frost was recorded by observation.

  The test piece was exposed to the environment of the laboratory at about 25 ° C. and a relative humidity of about 70% RH while being moved from the thermostatic chamber 1 to the thermostatic chamber 2, so that the test piece was absorbed before moving into the second chamber.・ Condensation / frost has formed on the sample.

  In addition, in the first chamber, since the door of the tank at −10 ° C. was opened to the laboratory side, dew condensation and frost occurred in the structure in the tank and the temperature / humidity sensor, and the equipment and sensors deteriorated. It was not possible to repeat stable experiments.

  In the second chamber, when the door of the 0 ° C. tank was opened to the laboratory side, dew condensation occurred in the structure inside the tank and the temperature and humidity sensor, and the temperature and humidity control by feedback of the temperature and humidity sensor value was performed. I can't do it temporarily. Moreover, the temperature and humidity environment in the tank was once collapsed by the exchange of air between the laboratory and the tank.

  The above-mentioned various problems in the experimental procedure resulted in variations in the experimental data, and it was not possible to evaluate the moisture absorption / release characteristics.

  The moisture absorption and desorption amount measuring device and the moisture absorption and desorption amount measuring method according to the present invention are not limited to the above-described embodiment, and can be appropriately modified and implemented without departing from the gist of the present invention.

  10, 20: moisture absorption and desorption amount measuring device, 11: first chamber, 12: second chamber, 13: moving means, 14: passage, 15: shutter, 16: mass measuring means, 21: third chamber , 22 ... mass measuring means, 23 ... lifter, 31 ... dew condensation and frost detecting means

Claims (17)

Adapting the hygroscopic sample to a first atmosphere having a predetermined temperature and humidity;
Moving the hygroscopic sample adapted to the first atmosphere to a second atmosphere having at least one of a temperature and a humidity different from the first atmosphere;
In the second atmosphere, the mass of the hygroscopic sample is measured over time,
A method for measuring the amount of absorbed and released moisture, characterized in that:   2. The moisture absorption / release according to claim 1, wherein, when moving from the first atmosphere to the second atmosphere, the hygroscopic sample is held in a third atmosphere having a predetermined temperature and humidity. 3. Quantity measurement method.   The method according to claim 2, wherein the third atmosphere is a condition capable of maintaining a dry state or a wet state of the hygroscopic sample.   The method for measuring moisture absorption and desorption according to claim 2 or 3, wherein the third atmosphere is made to have the same conditions as the first atmosphere.   The method according to any one of claims 1 to 4, wherein a temperature (T1) of the first atmosphere is lower than a second dew point temperature (D2) in the second atmosphere.   The method according to any one of claims 1 to 4, wherein a temperature (T1) of the first atmosphere is higher than a second dew point temperature (D2) in the second atmosphere.   The method for measuring moisture absorption and desorption according to any one of claims 1 to 6, wherein at the same time as measuring the mass of the hygroscopic sample, the state of dew condensation or frost formation on the hygroscopic sample is detected.   The method for measuring moisture absorption and desorption according to any one of claims 1 to 7, wherein the hygroscopic sample is glass having a surface having an antifogging film.   The method according to any one of claims 1 to 8, wherein a part of the hygroscopic sample is coated with a material capable of suppressing a change due to atmospheric conditions. A first chamber capable of holding the inside thereof in a first atmosphere having a predetermined temperature and humidity;
A second chamber capable of holding the inside thereof in a second atmosphere different in at least one of temperature and humidity from the first atmosphere;
Moving means for moving the hygroscopic sample from the first chamber to the second chamber;
Mass measuring means provided in the second chamber;
An apparatus for measuring the amount of moisture absorbed and released, comprising:   When moving the hygroscopic sample from the first chamber to the second chamber, a third type that can accommodate the hygroscopic sample and hold the sample in a third atmosphere having a predetermined temperature and humidity. The moisture absorption and desorption amount measurement device according to claim 10, comprising:   The moisture absorption and desorption amount measuring device according to claim 10 or 11, further comprising a detecting unit in the second chamber, which can detect a state of dew condensation or frost formation in the hygroscopic sample.   13. The apparatus according to claim 10, wherein at least one of the first chamber and the second chamber has a first temperature / humidity adjusting unit for adjusting temperature and humidity in an atmosphere in the chamber. Moisture absorption / desorption measurement device. The first chamber and the second chamber are disposed adjacent to each other;
The moisture absorption and desorption according to any one of claims 11 to 13, wherein the third chamber is a container that is movable from the first chamber to the second chamber while containing the hygroscopic sample. Quantity measuring device. The first chamber and the second chamber are spaced apart from each other;
The moisture absorption and desorption amount measurement device according to any one of claims 11 to 13, wherein the third chamber is a passage connecting the first chamber and the second chamber. A first shutter that partitions the passage and the first chamber;
A second shutter that partitions the passage and the second chamber;
Control means for controlling opening and closing of the first shutter and the second shutter at a desired timing;
The moisture absorption and desorption amount measuring device according to claim 15, comprising:   17. The moisture absorption / desorption measuring device according to claim 15, wherein the passage has second temperature / humidity adjusting means for independently adjusting the temperature and humidity of the internal atmosphere.

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