TW510965B - Humidity sensing material and method of preparing the humidity sensing material - Google Patents

Abstract

This invention discloses a humidity sensing material, which is composed of polymeric material of silane-modified 2-acrylamido-2-methyl-propane sulfonic acid. The humidity sensing material is prepared by hydrolyzing silane to Si(OH)4; adding Si(OH)4 to 2-acrylamido-2-methyl-propane sulfonic acid to yield a mixture by copolymerization; and thermally treating the mixture to form a film. According to the present invention, the humidity sensing material has the ability to avoid performance degradation under high humidity atmosphere, in addition to good stability, consistent humidity-sensing characteristics, and wide humidity-sensing range.

Description

V. Description of the invention (1) The present invention relates to a polymer material for the porous structure of a humidity sensor for a humidity sensor. It is particularly relevant to the potential of a humidity sensor in the field of modern life. > Μ ... There is an increasingly important trend; Γ Environmental control or agricultural facilities and other fields are known for humidity sensing materials can be divided into ⑴ electrolytic Wu (2) Jing Ye, ceramics (3) polymer materials, etc. . The advantages of measuring dense ceramics are high stability and good heat resistance. However, it is very difficult to use gold. The hysteresis phenomenon of K-knife in porous ceramics is more obvious. The characteristics of ί Γ (Γgan hydrophilic polymer, because of its good humidity sensing S2H materials such as rhenium, electrolyte (LiC1), etc. are more commonly used as :: J 土 测 材 枓. But this type of hydrophilicity is high When the molecular material is placed in the second year of high school, it will peel off from the substrate or electrode due to its good water absorption characteristics, which will cause the shirt material to swell or shrink. Detect degradation phenomena such as linear offset and poor qualitative characteristics. Currently, hydrophilic polymers used in humidity sensing materials, such as 2-propanamido-2-methylpropanesulfonic acid (AMPS), In the environment, there will be the disadvantages of dissolution and peeling, which will cause the bias of the sensing linearity, as shown in Figure 1, which represents the normal operating conditions, and □ represents the deviation of the sensing performance under high humidity. The problem, related patents are US Patent No. 4473813 which uses a protective layer to cover the hydrophilic high-knife sensing layer, or, for example, Sakai et al. (Sensors and

Actuators B, 13-14 (1993) 82. and Sensors and

Actuators β, 35-36 (1 996) 85.) Using two methods, one is to

0729-7242TWf; 07900014; Phoebe.ptd 510965 V. Description of the invention (2) Hydrophilic polymers are grafted on non-hydrophilic high-molecular-weight polymers and non-hydrophilic μ λ ^ i. The second is to pass the parent phase through the polymer Reticulated system (interpene, combined way to form an inter-network; IPN) structure to achieve 1ng resistance requires more complex chemical synthesis and control conditions' & the above-mentioned method is to provide a novel humidity sensing material by invention, Basin (Lrm machine materials are mixed in a simple single-step method eight (H = d: d, that is,…) 'Using a simple oven heat treatment side ί consistent humidity sensing characteristics, with a wide range of humidity sensing' I in Humidity-sensing material that is not damaged under the range of 冋 1 degree target. 2 Invented the invention, Mingzhi humidity-sensing material is composed of 2-propionamido-2-methylpropanesulfonic acid with Shixim Polymer material 'The above-mentioned silanes suitable for the humidity sensing material of the present invention are those which can be obtained by hydrolysis. Μ 7 π system is a method for preparing the above-mentioned humidity sensing material by hydrolysis, including: Class ς solution. Into ⑽ or ㈣2; add people 2-propyl amine 2-Methylpropionic acid is obtained in Si ° to obtain a mixture; and the above mixture is screen-printed into a film and heat-treated in a phase heating manner. The content of the hydrolyzed silanes is preferably less than 16.25 (% W / W), and the above heat treatment is preferably an oven for heating, and the temperature of the oven is set to two stages, where the first stage is 9 (rc, and the first stage is 180 ° C. As for the heating time, the first The heating time in one stage is preferably 3 to 5 minutes, and the heating time in the second stage is preferably 810 minutes. In addition, the reaction temperature for performing the polymerization reaction is preferably higher than

510965 V. Description of the invention (3) 90 ° C. After 2-propanamido-2-methylpropanesulfonic acid (AMPS) is modified with hydroalkanes, it can increase the resistance of the prepared humidity sensing material. In addition, in order to maintain its hygroscopicity, it is ideal Within the range, the addition of triethyl amine (TEA) or diethyl amine (dimethyl amine; DEA), among which TEA has the better effect. According to the humidity sensing material of the present invention, a thick film humidity sensor can be used. The humidity sensor can not only improve the deterioration phenomenon of the material in a high humidity environment, but also has good longevity. In order to keep the above-mentioned objects and features of the present invention, the preferred embodiments are listed below in order to cooperate with all of the following. 易 1 · < 'Below: σ The drawings are not detailed. The description is as a simple diagram: Figure 1 shows the traditional 2 ~ propylammonium (AMPS) and the sensation under the propyl propionate script environment and high humidity environment according to the embodiment of the present invention ^ = ㈣ humidity sensor In general, the second diagram is shown at 15 ° C, 25, and π. The humidity sensing material of the embodiment of the present invention is tested at the ambient temperature of $ C%. FIG. 3 is a graph showing the characteristic curve of the present invention. Graph of the sensing characteristics. ^ Comparative Example Humidity Sensing Material Muxigu 1 Gel paste does not fish for the difference of tender flashes ^ "Long-term stability. Fig. 5 shows that 4 ^^ in Examples 1 to 3

T added triethylamine (TEA

i〇% 5 Description of the Invention (4)-Figure 6 of Yiying & Amine (DEA) and the humidity sensing material without adding the above compounds is a graph showing the hysteresis phenomenon according to the present invention g & a, ηί Ming ^ Example 1 The hydration-sensing material prepared in Example 1 is used. Example 1 Hydrolyzed tetraethyloxanite (TEOs) is added to 2-propanamine based on μ Λ propionite fulvic acid and 0.4ml. Copolymerization reaction of triethylamine (tea), heated to high temperature for at least 1 hour to form an inorganic and silicon-containing porous structure humidity sensing material, in which tetraethyl A gas: : Tim, the amount is 16.25% (w / w). The prepared humidity sensing material = method is printed on an alumina substrate having a pair of comb electrodes. Then, the humidity sensing element is added to an oven (oven) plus square 4; the temperature and time of the flood box are divided into two sections: the first section is 9. With 'bell' and the second segment is 180t 8 ~ 10 minutes. 5 knives Example 2 = Diethylamine (DEA) was used instead of the triethylamine in Example 1. The other conditions were kept constant to prepare a humidity sensing material. Formula of Example 3: Except for Cethylamine (TEA) 'The same as Example 1 was used to prepare a humidity sensing material. Comparative Example The heating method in Example i was replaced with a hot piate heating method, and other conditions remained unchanged. " 9 σ

Ming 65 V. Description of the invention (5) 2. After the humidity sensing elements prepared in the above embodiments are tested, the following measurements are performed.

Formula I 1 · High humidity resistance ·· As shown in Figure 1, the test performance described above is biased. After being placed in a high humidity environment, the test performance curve changes from □ i to TE0S in this embodiment. In the modified (AMPS), φ indicates that the system is in operation and 〇 indicates that it is both in a high-humidity environment. Therefore, the humidity sensing material of the present invention can still maintain its test performance in a high-humidity environment. Measurement: Ambient temperature effect: At the ambient temperature of 15 ° c, 25 ° c, 35 ° c, β "Sensing characteristics of humidity sensing materials' as shown in Figure 2, Lizhong ^ ——," The axis is relative Humidity has three kinds of axes = measurement: the property is almost heavy 4, so the humidity sensing material of the present invention still maintains its sensing characteristics at different temperatures. Material Λ if Γπ: Take the humidity of Example 1 and Comparative Example Sensing material basin fruit: Does the Jr 丄 method affect the humidity sensing material,

The axis is H: jin indicates that ′ represents an oven; • represents a heating plate, in which the Y 3rd Η 吾 1Γ: anCe) ′ and the X-axis is relative humidity (% RH). From Figure 3, it can be seen that the sensing material with the hot plate plus 埶 method has a long humidity measurement 'for the box to be made 0 0571χ + 7' 0, the linearity curve is Y = -0 Degree Γ is good 3 'and only 2 is 0.9989, its value is very close to i, indicating linearity 5 · long-term stability at relative humidity (RH) 30%, 60

V. Description of the invention ⑹% > Q Π 〇 / u% In a humidity environment, the impedance value of the humidity sensing material prepared in Example 1 was continuously tested for 3 consecutive days, as shown in Figure 4, where ▲ Lufen ^ Represents relative humidity (RH) 30%, 60%, 90%.

Ml 4t I #! 7 Human differences, so the humidity-sensing material of the present invention does have a stable # ′ that does not deteriorate due to the increase in use time. 6. Wet phenomenon: Figure 5 shows the effects of adding triethylamine A), diethylamine (DEA), and not adding the above compounds on the humidity sensing material in Examples 1 to 3. In the figure, # / 〇 indicates the dehumidification and dehumidification test of TEA added in Example 1; ▲ / △ indicates the dehumidification and dehumidification test of DEA added in Example 2; / □ dehumidification test of Example 3 As well as liter test. It can be seen that the moisture sensitivity ranges of adding tea and dea are relative = degrees (RH) 40% ~ 90% and 50% ~ 90%. Among them, the addition of tea has a better effect of reducing hysteresis than A. The effect is that adding TEA can increase the humidity sensing range of the humidity sensing material. 〇? Hysteresis: From Figure 6, it can be seen that under the condition of adding 16.25% w / w) tetraethyloxysilane in Example 1, the deviation of the humidity test curve under the relative humidity (rh)% Only 2%, and has sufficient moisture resistance characteristics when the machine is 95% humidity (RH). Based on the above results, it can be seen that the use of the humidity sensing material of the present invention avoids: Ϊ ί: The humidity sensor made by the method can not only improve the humidity resistance = the deterioration phenomenon in a wet environment, even after a long time Γ The energy is still maintained in an excellent state, and it still has a good sense in a good stable temperature range. The Tezino field cannot be fed. The humidity sensing material of the present invention will not be affected by the test environment.

510965 V. Description of the invention (7) Temperature and humidity affect its sensing performance, thus reaching the invention level. Although the present invention has been disclosed as above with preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications and retouching without departing from the spirit and scope of the present invention. Therefore, the present invention The scope of protection shall be determined by the scope of the attached patent application.

0729-llAim; 07900014; Phoebe. P t d p. 10

Claims (1)

510965 VI. Scope of Patent Application 1. A humidity sensing material, which is a polymer material composed of 2-propane modified by silanes, of which amino-2-methylpropanesulfonic acid. 2 · Humidity sensing material as described in item 1 of the patent application range The silanes are hydrolyzable to Si (0H) 4. 3 · The humidity-sensing material described in item 2 of the patent application scope The hydrolyzed silane content is less than 16.25% (W / W) ° 4 · The humidity-sensing material described in item 1 of the patent application scope also Including triethylamine or diethylamine. 5 · A method for preparing a humidity sensing material, comprising: a · hydrolyzing silanes to Si (〇H) 4; b · adding hydrolyzed si (〇H) 4 to 2-propanamido-2 -Mixing and copolymerizing in methylpropanesulfonic acid to obtain a mixture; and c. Forming a film of said mixture by heat treatment. 6. The method for preparing a humidity-sensing material according to item 5 of the scope of patent application, wherein step b further comprises adding triethylamine or diethylamine. 7 · The method for preparing a humidity sensing material as described in item 5 of the scope of the patent application ', wherein after hydrolysis, the content of ε-yakis is less than 16.25% (W / W). 8. The method for preparing a humidity sensing material as described in item 5 of the patent application scope, wherein the heat treatment is performed by oven heating. 9. The method for preparing a humidity-sensing material as described in item 7 of the scope of the patent application, wherein the temperature of the oven is set to two stages, wherein the first stage is 90 ° C and the second stage is 180 °. 1 〇 The method for preparing a humidity sensing material as described in Item 8 of the scope of the patent application, wherein the heating time is 3 to 5 minutes in the first stage of temperature, and 0729-7242HVf; 07900014; Phoebe.ptd 11th tribute 510965 0729-7242TWf; 07900014; Phoebe.p t d p. 12