CN107325472A - A kind of humidity sensing polymer materials and preparation method thereof - Google Patents
A kind of humidity sensing polymer materials and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of humidity sensing polymer materials and preparation method thereof.The humidity-sensitive material includes following components：Polyamic acid, polyethylene amidogen acid, sulfonated phenylethylene, 1-chloro-4-methyl-benzene, sodium carboxymethylcellulose pyce, polymethyl methacrylate, dodecyl sodium sulfate, cellulose acetate, polyethylene glycol, foam copper, nano silica fume, bamboo fibre, poly- 4 vinylpyridine, methanol, to dimethyl ethanedioic acid benzene methyl, deionized water, sorbierite, nano-sized carbon.After polyamic acid, polyethylene amidogen acid, sulfonated phenylethylene, 1-chloro-4-methyl-benzene, dodecyl sodium sulfate Hybrid Heating, then with polymethyl methacrylate, sodium carboxymethylcellulose pyce, dodecyl sodium sulfate, cellulose acetate, poly- 4 vinylpyridine, to after dimethyl ethanedioic acid benzene methyl Hybrid Heating freeze grind to obtain the second mixture；Finally with blown film after remaining component mixed grinding.Humidity-sensitive material stability of the present invention is good, and weatherability is strong, it is easy to preserve.
Description
Technical field
The invention belongs to semiconductor preparation field, and in particular to a kind of humidity sensing polymer materials and preparation method thereof.
Background technology
Humistor be cause resistance value itself to change using the moisture in humidity-sensitive material absorption air this is former
What reason was made.Humidity-sensitive material it is wet constitute humidity sensor important component, its performance directly affect sensor sensitivity,
Response speed, humidity hysteresis and sensor life-time etc..
The main excellent electrolytes of conventional humidity-sensitive material, high-molecular compound, ceramic based material, porous metals oxidation at present
Thing and semi-conducting material.The easy stream of electrolytic salt wherein in electrolytes material and be diluted, or even outflow, destroy material
Wet sensing performance, although ceramics and porous metal material are with excellent heat resistance, and response is rapid, its resistance temperature system
Number teaching, repeatability and interchangeability are poor, and not anti-pollution；Humidity sensing polymer materials are with its material source, RH range
Width, hysteresis is small, and the excellent properties such as fast response time have obtained increasing concern.
The Chinese patent of application number 201510069712.3 discloses a kind of polyimides humidity-sensitive material and preparation method thereof,
First by dianhydride, diamines, alcohol reagent, N, N'- DICs condensing agent, highly polar aprotic solvents A and strong
Polar aprotic solvents B prepares polyesteramide powder, and then polyesteramide powder is mixed with highly polar aprotic solvents C
Close, solidification is obtained；Described dianhydride and the mol ratio of diamines are 1:(0.85~1.1)；Described dianhydride and the matter of alcohol reagent
Amount is than being 1:(3~15)；Described dianhydride and the mol ratio of N, N'- DIC condensing agent are 1:(1~10)；Institute
The dianhydride stated and highly polar aprotic solvents A mass ratio are 1:(1~5)；Described dianhydride with it is highly polar non-protonated molten
Agent B mass ratio is 1:(1~10)；Described polyesteramide powder and highly polar aprotic solvents C mass ratio are 1:
(1.5~9)；When described dianhydride is 3,3', 4,4'- benzophenone tetracarboxylic dianhydrides or 4,4'- oxygen pair phthalic anhydride,
Described diamines is 2,2- double [4- (4- amino-benzene oxygens) phenyl] -1,1,1,3,3,3- HFC-236fas, (fluoroforms of 2,2'- bis-
Base) benzidine, 3,3'- bis- (trifluoromethyl) benzidine, double (4- aminophenyls) HFC-236fas of 2,2-, 2,2'- are double
(trifluoromethyl) -4,4'- diamino-phenyls ether or 4,4'- [1,4- phenyl is double (oxygen)] double [3- (trifluoromethyl) aniline]；Work as institute
When the dianhydride stated is 4,4'- (hexafluoro isopropyl alkene) two anhydride phthalic acid, described diamines is double [4- (4- amino-benzene oxygens) benzene of 2,2-
Base] -1,1,1,3,3,3- HFC-236fas, double (the trifluoromethyl) -4,4'- diamino-phenyls ethers of 2,2'-, (the 4- aminobenzenes of 4,4'- bis-
Epoxide) biphenyl, 3,4'- diaminodiphenyl ethers, double (3- amino-benzene oxygens) benzene of 1,3-, double (4'- amino-benzene oxygens) benzene of 1,3- or
Double (4- amino-benzene oxygens) benzene of 1,4-.Polyimides humidity-sensitive material prepared by the present invention, its precursor is with more excellent storage
Deposit after the polyesteramide of stability and anti-hydrolytic performance, solidification that polyimides humidity sensitive thin film humidity hysteresis is smaller, the linearity is good, high green end
It is stable, without compensation, have a good application prospect.
Chinese invention patent CN103467983A disclose it is a kind of for high-altitude humidity detect Kapton and its
Preparation method, the Kapton is absorption and abjection hydrone speed as obtained from polyamic acid high temperature imidizate
It hurry up, moisture sensitivity is high.But the precursor polyamic acid of polyimides is easily hydrolyzed and dropped due to the presence of its carboxyl
Solution, bin stability is poor.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of humidity sensing polymer materials and its preparation side
Method, the humidity-sensitive material performance is stable, and weatherability is strong, is quick on the draw, it is easy to store.
For prior art problem, the technical scheme that the present invention takes is：
A kind of humidity sensing polymer materials, including the following component counted by weight：46-65 parts of polyamic acid, polyethylene amino
25-44 parts of Amino acid, 44-88 parts of sulfonated phenylethylene, 18-44 parts of 1-chloro-4-methyl-benzene, 29-42 parts of sodium carboxymethylcellulose pyce, poly- first
38-58 parts of base methyl acrylate, 22-44 parts of dodecyl sodium sulfate, 12-28 parts of cellulose acetate, 28-55 parts of polyethylene glycol,
24-53 parts of foam copper, 1-9 parts of nano silica fume, 2-9 parts of bamboo fibre, poly- 4-vinylpyridine 8-22 parts, 15-38 parts of methanol, to diformazan
1-9 parts of base ethanedioic acid benzene methyl, 1-9 parts of deionized water, 0.1-0.8 parts of sorbierite, 18-42 parts of nano-sized carbon.
It is as improved, above-mentioned humidity sensing polymer materials, including the following component counted by weight：Polyamic acid 56
Part, 42 parts of polyethylene amidogen acid, 64 parts of sulfonated phenylethylene, 36 parts of 1-chloro-4-methyl-benzene, 37 parts of sodium carboxymethylcellulose pyce, poly- first
50 parts of base methyl acrylate, 34 parts of dodecyl sodium sulfate, 25 parts of cellulose acetate, 37 parts of polyethylene glycol, 41 parts of foam copper is received
6 parts of silica flour of rice, 7 parts of bamboo fibre, poly- 14 parts of 4-vinylpyridine, 27 parts of methanol, to 4 parts of dimethyl ethanedioic acid benzene methyl, deionization
8 parts of water, 0.2 part of sorbierite, 31 parts of nano-sized carbon.
It is as improved, described nano silica fume 20-60 microns.
The preparation method of above-mentioned humidity sensing polymer materials, comprises the following steps：Step 1, each component is weighed；Step 2, will be poly-
In amic acid, polyethylene amidogen acid, sulfonated phenylethylene, 1-chloro-4-methyl-benzene, dodecyl sodium sulfate input reactor, plus
Hot to 340-520 DEG C obtains the first mixture；Step 2, by the first mixture, polymethyl methacrylate, sodium carboxymethylcellulose pyce, ten
Dialkyl sulfonates, cellulose acetate, poly- 4-vinylpyridine, to dimethyl ethanedioic acid benzene methyl put into reactor in, be heated to
120-140 DEG C, put into ultra low temperature freezer, it is lyophilized to grind to obtain the second mixture；Step 3, by the second mixture, foam copper, receive
After being ground in rice silica flour, carbon fiber, methanol, nano-sized carbon, deionized water, sorbierite input ball mill, input inflation film manufacturing machine blowout is thick
Spend the humidity-sensitive material for 10-20 microns.
It is that the degree of cross linking of second mixture is 72.5-81.4% in step 2 as improved.
It is that the blown film temperature of inflation film manufacturing machine is 100-120 DEG C in step 3 as improved.
Beneficial effect
Humidity sensing polymer materials reaction speed of the present invention is fast, and weatherability is strong, and stability is good, and the humidity sensing polymer materials of preparation are easy to
Preserve, in addition, the mixing of bamboo fibre and nano silica fume, improves the stability and reaction speed of material.
Embodiment
Embodiment 1
A kind of humidity sensing polymer materials, including the following component counted by weight：46 parts of polyamic acid, polyethylene amidogen
25 parts of acid, 44 parts of sulfonated phenylethylene, 18 parts of 1-chloro-4-methyl-benzene, 29 parts of sodium carboxymethylcellulose pyce, 38 parts of polymethyl methacrylate,
22 parts of dodecyl sodium sulfate, 12 parts of cellulose acetate, 28 parts of polyethylene glycol, 24-53 parts of foam copper, 1 part of nano silica fume, bamboo is fine
2-9 parts of dimension, poly- 8 parts of 4-vinylpyridine, 15 parts of methanol, to 1 part of dimethyl ethanedioic acid benzene methyl, 1-9 parts of deionized water, sorbierite
0.1 part, 18 parts of nano-sized carbon.
20 microns of the nano silica fume.
The preparation method of above-mentioned humidity sensing polymer materials, comprises the following steps：Step 1, each component is weighed；Step 2, will be poly-
In amic acid, polyethylene amidogen acid, sulfonated phenylethylene, 1-chloro-4-methyl-benzene, dodecyl sodium sulfate input reactor, plus
Hot to 340 DEG C obtain the first mixture；Step 2, by the first mixture, polymethyl methacrylate, sodium carboxymethylcellulose pyce, dodecane
Base sodium sulfonate, cellulose acetate, poly- 4-vinylpyridine, to dimethyl ethanedioic acid benzene methyl put into reactor in, be heated to 120
DEG C, it is lyophilized to grind to obtain the second mixture in input ultra low temperature freezer；Step 3, by the second mixture, foam copper, nano silica fume,
After being ground in carbon fiber, methanol, nano-sized carbon, deionized water, sorbierite input ball mill, input inflation film manufacturing machine blowout thickness is 10 micro-
The humidity-sensitive material of rice.
The degree of cross linking of second mixture is 72.5% in step 2.
The blown film temperature of inflation film manufacturing machine is 100 DEG C in step 3.
Embodiment 2
A kind of humidity sensing polymer materials, including the following component counted by weight：56 parts of polyamic acid, polyethylene amidogen
42 parts of acid, 64 parts of sulfonated phenylethylene, 36 parts of 1-chloro-4-methyl-benzene, 37 parts of sodium carboxymethylcellulose pyce, 50 parts of polymethyl methacrylate,
34 parts of dodecyl sodium sulfate, 25 parts of cellulose acetate, 37 parts of polyethylene glycol, 41 parts of foam copper, 6 parts of nano silica fume, bamboo fibre 7
Part, poly- 14 parts of 4-vinylpyridine, 27 parts of methanol, to 4 parts of dimethyl ethanedioic acid benzene methyl, 8 parts of deionized water, 0.2 part of sorbierite,
31 parts of nano-sized carbon.
50 microns of the nano silica fume.
The preparation method of above-mentioned humidity sensing polymer materials, comprises the following steps：Step 1, each component is weighed；Step 2, will be poly-
In amic acid, polyethylene amidogen acid, sulfonated phenylethylene, 1-chloro-4-methyl-benzene, dodecyl sodium sulfate input reactor, plus
Hot to 480 DEG C obtain the first mixture；Step 2, by the first mixture, polymethyl methacrylate, sodium carboxymethylcellulose pyce, dodecane
Base sodium sulfonate, cellulose acetate, poly- 4-vinylpyridine, to dimethyl ethanedioic acid benzene methyl put into reactor in, be heated to 130
DEG C, it is lyophilized to grind to obtain the second mixture in input ultra low temperature freezer；Step 3, by the second mixture, foam copper, nano silica fume,
After being ground in carbon fiber, methanol, nano-sized carbon, deionized water, sorbierite input ball mill, input inflation film manufacturing machine blowout thickness is 15 micro-
The humidity-sensitive material of rice.
The degree of cross linking of second mixture is 75.4% in step 2.
The blown film temperature of inflation film manufacturing machine is 108 DEG C in step 3.
Embodiment 3
A kind of humidity sensing polymer materials, including the following component counted by weight：46-65 parts of polyamic acid, polyethylene amino
25-44 parts of Amino acid, 44-88 parts of sulfonated phenylethylene, 18-44 parts of 1-chloro-4-methyl-benzene, 29-42 parts of sodium carboxymethylcellulose pyce, poly- first
38-58 parts of base methyl acrylate, 22-44 parts of dodecyl sodium sulfate, 12-28 parts of cellulose acetate, 28-55 parts of polyethylene glycol,
24-53 parts of foam copper, 1-9 parts of nano silica fume, 2-9 parts of bamboo fibre, poly- 4-vinylpyridine 8-22 parts, 15-38 parts of methanol, to diformazan
1-9 parts of base ethanedioic acid benzene methyl, 1-9 parts of deionized water, 0.1-0.8 parts of sorbierite, 18-42 parts of nano-sized carbon.
60 microns of the nano silica fume.
The preparation method of above-mentioned humidity sensing polymer materials, comprises the following steps：Step 1, each component is weighed；Step 2, will be poly-
In amic acid, polyethylene amidogen acid, sulfonated phenylethylene, 1-chloro-4-methyl-benzene, dodecyl sodium sulfate input reactor, plus
Hot to 520 DEG C obtain the first mixture；Step 2, by the first mixture, polymethyl methacrylate, sodium carboxymethylcellulose pyce, dodecane
Base sodium sulfonate, cellulose acetate, poly- 4-vinylpyridine, to dimethyl ethanedioic acid benzene methyl put into reactor in, be heated to 140
DEG C, it is lyophilized to grind to obtain the second mixture in input ultra low temperature freezer；Step 3, by the second mixture, foam copper, nano silica fume,
After being ground in carbon fiber, methanol, nano-sized carbon, deionized water, sorbierite input ball mill, input inflation film manufacturing machine blowout thickness is 20 micro-
The humidity-sensitive material of rice.
The degree of cross linking of second mixture is 81.4% in step 2.
The blown film temperature of inflation film manufacturing machine is 120 DEG C in step 3.
Embodiment 4
A kind of humidity sensing polymer materials, including the following component counted by weight：56 parts of polyamic acid, polyethylene amidogen
42 parts of acid, 64 parts of sulfonated phenylethylene, 36 parts of 1-chloro-4-methyl-benzene, 37 parts of sodium carboxymethylcellulose pyce, 50 parts of polymethyl methacrylate,
34 parts of dodecyl sodium sulfate, 25 parts of cellulose acetate, 37 parts of polyethylene glycol, 41 parts of foam copper, 6 parts of nano silica fume, bamboo fibre 7
Part, poly- 14 parts of 4-vinylpyridine, 27 parts of methanol, to 4 parts of dimethyl ethanedioic acid benzene methyl, 8 parts of deionized water, 0.2 part of sorbierite,
31 parts of nano-sized carbon.
50 microns of the nano silica fume.
The preparation method of above-mentioned humidity sensing polymer materials, comprises the following steps：Step 1, each component is weighed；Step 2, will be poly-
Amic acid, polyethylene amidogen acid, sulfonated phenylethylene, 1-chloro-4-methyl-benzene, dodecyl sodium sulfate, poly-methyl methacrylate
Ester, sodium carboxymethylcellulose pyce, dodecyl sodium sulfate, cellulose acetate, poly- 4-vinylpyridine, to dimethyl ethanedioic acid benzene methyl throw
Enter in reactor, be heated in 130 DEG C, input ultra low temperature freezer, it is lyophilized to grind to obtain the second mixture；Step 2, by the second mixing
After being ground in thing, foam copper, nano silica fume, carbon fiber, methanol, nano-sized carbon, deionized water, sorbierite input ball mill, input
Inflation film manufacturing machine blowout thickness is 15 microns of humidity-sensitive material.
The degree of cross linking of second mixture is 75.4% in step 2.
The blown film temperature of inflation film manufacturing machine is 108 DEG C in step 2.
Embodiment 5
In addition to bamboo fibre is not contained, other be the same as Examples 2.
Embodiment 6
In addition to without nano silica fume, other be the same as Examples 2.
Performance test
To the performance detection of the embodiment 1-7 humidity-sensitive materials prepared, the data obtained is as shown in the table.
It is seen from the above data that the humidity-sensitive material reaction time of the present invention is short, recover fast, sensitivity is high, improves existing height
The unstability of molecule humidity-sensitive material, extends the preservation time.And comparative example 2 and embodiment 4 are understood, substep mixing group
Point, the harmonious ability between component is improved, reaction time, water absorption rate and the sensitivity of humidity sensing polymer materials is improved, compares
Knowable to embodiment 2, comparative example 5-7, heat-resist, the combination property height of humidity-sensitive material of the present invention.
Claims (6)
1. a kind of humidity sensing polymer materials, it is characterised in that including the following component counted by weight：Polyamic acid 46-65
Part, 25-44 parts of polyethylene amidogen acid, 44-88 parts of sulfonated phenylethylene, 18-44 parts of 1-chloro-4-methyl-benzene, sodium carboxymethylcellulose pyce
29-42 parts, 38-58 parts of polymethyl methacrylate, 22-44 parts of dodecyl sodium sulfate, 12-28 parts of cellulose acetate, poly- second
28-55 parts of glycol, 24-53 parts of foam copper, 1-9 parts of nano silica fume, 2-9 parts of bamboo fibre, poly- 4-vinylpyridine 8-22 parts, methanol
15-38 parts, to 1-9 parts of dimethyl ethanedioic acid benzene methyl, 1-9 parts of deionized water, 0.1-0.8 parts of sorbierite, nano-sized carbon 18-42
Part.
2. a kind of humidity sensing polymer materials according to claim 1, it is characterised in that counted by weight including following
Component：56 parts of polyamic acid, 42 parts of polyethylene amidogen acid, 64 parts of sulfonated phenylethylene, 36 parts of 1-chloro-4-methyl-benzene, methyl is fine
Plain 37 parts of the sodium of dimension, 50 parts of polymethyl methacrylate, 34 parts of dodecyl sodium sulfate, 25 parts of cellulose acetate, polyethylene glycol 37
Part, 41 parts of foam copper, 6 parts of nano silica fume, 7 parts of bamboo fibre, poly- 14 parts of 4-vinylpyridine, 27 parts of methanol, to dimethyl ethanedioic acid
4 parts of benzene methyl, 8 parts of deionized water, 0.2 part of sorbierite, 31 parts of nano-sized carbon.
3. a kind of humidity sensing polymer materials according to claim 1, it is characterised in that described nano silica fume 20-60 microns.
4. the preparation method based on any humidity sensing polymer materials of claim 1-3, it is characterised in that comprise the following steps：
Step 1, each component is weighed；Step 2, by polyamic acid, polyethylene amidogen acid, sulfonated phenylethylene, 1-chloro-4-methyl-benzene, ten
In dialkyl sulfonates input reactor, it is heated to 340-520 DEG C and obtains the first mixture；Step 2, by the first mixture, poly- first
Base methyl acrylate, sodium carboxymethylcellulose pyce, dodecyl sodium sulfate, cellulose acetate, poly- 4-vinylpyridine, to dimethyl second two
In sour benzene methyl input reactor, it is heated in 120-140 DEG C, input ultra low temperature freezer, it is lyophilized to grind to obtain the second mixture；Step
Rapid 3, the second mixture, foam copper, nano silica fume, carbon fiber, methanol, nano-sized carbon, deionized water, sorbierite are put into ball mill
In grind after, input inflation film manufacturing machine blowout thickness is 10-20 microns of humidity-sensitive material.
5. the preparation method of a kind of humidity sensing polymer materials according to claim 4, it is characterised in that second in step 2
The degree of cross linking of mixture is 72.5-81.4%.
6. a kind of preparation method of humidity sensing polymer materials according to claim 4, it is characterised in that blown film in step 3
The blown film temperature of machine is 100-120 DEG C.
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| US20210238392A1 (en) * | 2020-01-30 | 2021-08-05 | Fuji Xerox Co., Ltd. | Polyimide precursor-containing aqueous composition, method for producing polyimide film, and method for producing porous polyimide film |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592756A (en) * | 2015-02-10 | 2015-05-06 | 中国电子科技集团公司第四十九研究所 | Polyimide humidity-sensitive material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104592756A (en) * | 2015-02-10 | 2015-05-06 | 中国电子科技集团公司第四十九研究所 | Polyimide humidity-sensitive material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210238392A1 (en) * | 2020-01-30 | 2021-08-05 | Fuji Xerox Co., Ltd. | Polyimide precursor-containing aqueous composition, method for producing polyimide film, and method for producing porous polyimide film |
| US11680156B2 (en) * | 2020-01-30 | 2023-06-20 | Fujifilm Business Innovation Corp. | Polyimide precursor-containing aqueous composition, method for producing polyimide film, and method for producing porous polyimide film |
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Application publication date: 20171107 |