CN107389735A - A kind of preparation method of the humidity sensor based on molecular sieve - Google Patents
A kind of preparation method of the humidity sensor based on molecular sieve Download PDFInfo
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- CN107389735A CN107389735A CN201710361820.7A CN201710361820A CN107389735A CN 107389735 A CN107389735 A CN 107389735A CN 201710361820 A CN201710361820 A CN 201710361820A CN 107389735 A CN107389735 A CN 107389735A
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- molecular sieve
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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Abstract
The invention provides a kind of preparation method of the humidity sensor based on molecular sieve, first aluminium hydroxide is added in phosphate aqueous solution, heating stirring, Tri-n-Propylamine is added after cooling, continues to stir, places reaction liquid into autoclave and reacted, then gained white product is washed with deionized water only, dry, finally by gained molecular sieve and deionized water mixed grinding, coated on the Al based on Ag Pd interdigital electrodes2O3In ceramic substrate, aging, produce.Gained humidity sensor impedance variations scope of the invention is 3 orders of magnitude, and humidity hysteresis winding is less than 3%, and response recovery time is all preferable in 2 ~ 3s, response recovery characteristics.
Description
Technical field
The invention belongs to humidity sensor technical field, and in particular to a kind of preparation of the humidity sensor based on molecular sieve
Method.
Background technology
Molecular screen material refers to contain micropore of uniform size in material structure, and the diameter of these micropores can be with molecular diameter
Analogy.Molecular screen material is mainly characterized by the ionic species in porous, the different pore sizes and pore passage structure in structure
Difference, these features determine molecular sieve for the Selective adsorption of different molecular, screening or catalytic etc..People grind
Study carefully the synthesis of molecular screen material, making, the basis of application be all based on to molecular sieve internal structure duct understanding number, such as
Van der Waals force between the interior molecules of molecular sieve crystal hole and microcosmic internal field and coulomb interaction caused by the polarity of dipole
So that there is the characteristic of selective absorption for specific gas molecule or polar molecule, for another example the size diameter in aperture
General distribution is consistent, therefore the molecule only less than aperture can be just entered inside hole, or departs from hole easily, Huo Zheyong
Exist long in hole.Molecular screen material has desk study, but humidity sensor in terms of gas sensor, chemical environment purification
On application it is few, to find out its cause, the response recovery time of molecular screen material is not ideal.
The content of the invention
The technical problem of solution：It is an object of the invention to provide a kind of preparation side of the humidity sensor based on molecular sieve
Method, the humidity sensor have good response recovery characteristics.
Technical scheme：A kind of preparation method of the humidity sensor based on molecular sieve, comprises the following steps：
Step 1, aluminium hydroxide 5-10g is added in 10-15v/v% phosphate aqueous solutions 30-40mL, is heated to 30-40 DEG C, stirring
30-40min, 25 DEG C are cooled to, add Tri-n-Propylamine 3-7mL under agitation, continue to stir, obtain reaction solution；
Step 2, step 1 gained reaction solution is placed in autoclave and reacted, obtain white product；
Step 3, step 2 gained white product is washed with deionized water only, dries, obtain molecular sieve；
Step 4, by step 3 gained molecular sieve and deionized water in mass ratio 4：1 mixed grinding, coated on interdigital based on Ag-Pd
The Al of electrode2O3In ceramic substrate, aging, produce.
Further, 0.5-1wt.% glucose and 0.1-0.5wt.% dodecyls are also contained in the phosphate aqueous solution
Benzene sulfonic acid sodium salt.
Further, stirring is is stirred by ultrasonic in step 1, supersonic frequency 500-800w.
Further, in step 2 reaction temperature be 150-170 DEG C, time 15-20h.
Further, drying temperature is 40-50 DEG C in step 3.
Further, aging condition is alternating voltage 0.5V, frequency 100Hz, 12-15h in step 4.
Beneficial effect：Gained humidity sensor impedance variations scope of the invention is 3 orders of magnitude, and humidity hysteresis winding is less than 3%,
Response recovery time is all preferable in 2 ~ 3s, response recovery characteristics.
Embodiment
Embodiment 1
A kind of preparation method of the humidity sensor based on molecular sieve, comprises the following steps：
Step 1, aluminium hydroxide 5g is added in 10v/v% phosphate aqueous solutions 40mL, is heated to 30 DEG C, stirred 30min, be cooled to
25 DEG C, Tri-n-Propylamine 3mL is added under agitation, continues to stir, obtains reaction solution；
Step 2, step 1 gained reaction solution is placed in autoclave and reacted, obtain white product；
Step 3, step 2 gained white product is washed with deionized water only, dries, obtain molecular sieve；
Step 4, by step 3 gained molecular sieve and deionized water in mass ratio 4：1 mixed grinding, coated on interdigital based on Ag-Pd
The Al of electrode2O3In ceramic substrate, aging, produce.
Wherein, 0.5wt.% glucose and 0.1wt.% neopelexes are also contained in the phosphate aqueous solution；Step
Stirring is is stirred by ultrasonic in rapid 1, supersonic frequency 500w；In step 2 reaction temperature be 150 DEG C, time 20h；Done in step 3
Dry temperature is 40 DEG C；Aging condition is alternating voltage 0.5V, frequency 100Hz, 12-15h in step 4.
Embodiment 2
A kind of preparation method of the humidity sensor based on molecular sieve, comprises the following steps：
Step 1, aluminium hydroxide 7g is added in 12v/v% phosphate aqueous solutions 36mL, is heated to 35 DEG C, stirred 30min, be cooled to
25 DEG C, Tri-n-Propylamine 5mL is added under agitation, continues to stir, obtains reaction solution；
Step 2, step 1 gained reaction solution is placed in autoclave and reacted, obtain white product；
Step 3, step 2 gained white product is washed with deionized water only, dries, obtain molecular sieve；
Step 4, by step 3 gained molecular sieve and deionized water in mass ratio 4：1 mixed grinding, coated on interdigital based on Ag-Pd
The Al of electrode2O3In ceramic substrate, aging, produce.
Wherein, 0.7wt.% glucose and 0.2wt.% neopelexes are also contained in the phosphate aqueous solution；Step
Stirring is is stirred by ultrasonic in rapid 1, supersonic frequency 500w；In step 2 reaction temperature be 160 DEG C, time 20h；Done in step 3
Dry temperature is 50 DEG C；Aging condition is alternating voltage 0.5V, frequency 100Hz, 12-15h in step 4.
Embodiment 3
A kind of preparation method of the humidity sensor based on molecular sieve, comprises the following steps：
Step 1, aluminium hydroxide 8g is added in 14v/v% phosphate aqueous solutions 40mL, is heated to 35 DEG C, stirred 35min, be cooled to
25 DEG C, Tri-n-Propylamine 6mL is added under agitation, continues to stir, obtains reaction solution；
Step 2, step 1 gained reaction solution is placed in autoclave and reacted, obtain white product；
Step 3, step 2 gained white product is washed with deionized water only, dries, obtain molecular sieve；
Step 4, by step 3 gained molecular sieve and deionized water in mass ratio 4：1 mixed grinding, coated on interdigital based on Ag-Pd
The Al of electrode2O3In ceramic substrate, aging, produce.
Wherein, 0.5wt.% glucose and 0.1wt.% neopelexes are also contained in the phosphate aqueous solution；Step
Stirring is is stirred by ultrasonic in rapid 1, supersonic frequency 500w；In step 2 reaction temperature be 150 DEG C, time 20h；Done in step 3
Dry temperature is 40 DEG C；Aging condition is alternating voltage 0.5V, frequency 100Hz, 12-15h in step 4.
Embodiment 4
A kind of preparation method of the humidity sensor based on molecular sieve, comprises the following steps：
Step 1, aluminium hydroxide 10g is added in 15v/v% phosphate aqueous solutions 30mL, is heated to 40 DEG C, stirred 40min, be cooled to
25 DEG C, Tri-n-Propylamine 7mL is added under agitation, continues to stir, obtains reaction solution；
Step 2, step 1 gained reaction solution is placed in autoclave and reacted, obtain white product；
Step 3, step 2 gained white product is washed with deionized water only, dries, obtain molecular sieve；
Step 4, by step 3 gained molecular sieve and deionized water in mass ratio 4：1 mixed grinding, coated on interdigital based on Ag-Pd
The Al of electrode2O3In ceramic substrate, aging, produce.
Wherein, 1wt.% glucose and 0.5wt.% neopelexes are also contained in the phosphate aqueous solution；Step
Stirring is is stirred by ultrasonic in 1, supersonic frequency 800w；In step 2 reaction temperature be 170 DEG C, time 15h；Dried in step 3
Temperature is 50 DEG C；Aging condition is alternating voltage 0.5V, frequency 100Hz, 12-15h in step 4.
The Unordered system of above-mentioned humidity sensor is measured with 6500B series precision impedances analyzer, AC voltages are set to 0.5V, survey
The frequency of examination is 40Hz to 100kHz, tests different humidity environments respectively with six kinds of saturated salt solution LiCl, Mg Cl2、Mg
(NO3)2, NaCl, KCl and KNO3Represent, the relative humidity of this six kinds of saturated salt solutions is respectively 11%, 33%, 54%, 75%,
85% and 95% RH.
The result of test is that impedance variations scope is 3 orders of magnitude, and humidity hysteresis winding is less than 3%, response recovery time all 2 ~
3s, gained humidity sensor response recovery characteristics are preferable.
Claims (6)
- A kind of 1. preparation method of the humidity sensor based on molecular sieve, it is characterised in that：Comprise the following steps：Step 1, aluminium hydroxide 5-10g is added in 10-15v/v% phosphate aqueous solutions 30-40mL, is heated to 30-40 DEG C, stirring 30-40min, 25 DEG C are cooled to, add Tri-n-Propylamine 3-7mL under agitation, continue to stir, obtain reaction solution；Step 2, step 1 gained reaction solution is placed in autoclave and reacted, obtain white product；Step 3, step 2 gained white product is washed with deionized water only, dries, obtain molecular sieve；Step 4, by step 3 gained molecular sieve and deionized water in mass ratio 4：1 mixed grinding, coated on interdigital based on Ag-Pd The Al of electrode2O3In ceramic substrate, aging, produce.
- 2. the preparation method of the humidity sensor according to claim 1 based on molecular sieve, it is characterised in that：The phosphoric acid Also contain 0.5-1wt.% glucose and 0.1-0.5wt.% neopelexes in the aqueous solution.
- 3. the preparation method of the humidity sensor according to claim 1 based on molecular sieve, it is characterised in that：In step 1 Stir as ultrasonic agitation, supersonic frequency 500-800w.
- 4. the preparation method of the humidity sensor according to claim 1 based on molecular sieve, it is characterised in that：In step 2 Reaction temperature is 150-170 DEG C, time 15-20h.
- 5. the preparation method of the humidity sensor according to claim 1 based on molecular sieve, it is characterised in that：In step 3 Drying temperature is 40-50 DEG C.
- 6. the preparation method of the humidity sensor according to claim 1 based on molecular sieve, it is characterised in that：In step 4 Aging condition is alternating voltage 0.5V, frequency 100Hz, 12-15h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000028311A1 (en) * | 1998-11-06 | 2000-05-18 | E+E Elektronik Ges.Mbh | System for measuring humidity |
| CN101629927A (en) * | 2009-08-13 | 2010-01-20 | 上海交通大学 | Porous aluminum oxide film humidity-dependent sensor preparation method |
| CN102175755A (en) * | 2011-02-16 | 2011-09-07 | 西安交通大学 | A carbon nanotube film micro-nano ionization sensor and its preparation method |
| CN103439368A (en) * | 2013-09-16 | 2013-12-11 | 吉林大学 | Phosphate molecular sieve based humidity sensor and preparation method thereof |
-
2017
- 2017-05-22 CN CN201710361820.7A patent/CN107389735A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000028311A1 (en) * | 1998-11-06 | 2000-05-18 | E+E Elektronik Ges.Mbh | System for measuring humidity |
| CN101629927A (en) * | 2009-08-13 | 2010-01-20 | 上海交通大学 | Porous aluminum oxide film humidity-dependent sensor preparation method |
| CN102175755A (en) * | 2011-02-16 | 2011-09-07 | 西安交通大学 | A carbon nanotube film micro-nano ionization sensor and its preparation method |
| CN103439368A (en) * | 2013-09-16 | 2013-12-11 | 吉林大学 | Phosphate molecular sieve based humidity sensor and preparation method thereof |
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