CN102967634A - Capacitive humidity-sensitive sensor based on anodic alumina film coplanar electrode structure and preparation method thereof - Google Patents
Capacitive humidity-sensitive sensor based on anodic alumina film coplanar electrode structure and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a capacitive humidity-sensitive sensor based on an anodic alumina film coplanar electrode structure. The capacitive humidity-sensitive sensor comprises an insulating substrate, a pair of coplanar electrode structure electrode layers positioned on the surface of the insulating substrate, and a sensitive layer positioned on one end of the coplanar electrode structure electrode layer. The invention also discloses a method for manufacturing the capacitive humidity-sensitive sensor based on the anodic alumina film coplanar electrode structure. The preparation method is simple and reliable, can be compatible with the conventional micro-electronic mechanical process, is suitable for batch production, and develops a wide prospect for the application of the humidity-sensitive sensor. In addition, the electrode structure is directly deposited on the surface of an insulating matrix and is positioned below the anodic alumina sensor, and the defects that the effective area is reduced as the electrode in the conventional capacitive humidity-sensitive sensor has a porous structure are overcome, so that the sensitivity is improved.
Description
Technical field
The present invention relates to electric capacity moisture sensor field, especially a kind of electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure and preparation method thereof.
Background technology
Moisture sensor has in fields such as food, medical treatment, agricultural, industry widely to be used, and compares with moisture sensors such as resistor-type, mass type, impedance types, and the capacitor type moisture sensor has the advantages such as response block, hysteresis quality are little, good stability.Nano-porous materials has large specific surface area, the surface exists a large amount of outstanding keys and surface imperfection isoreactivity center etc., and water vapor is very responsive in the environment to external world, has been widely used as sensitive material in the moisture sensor.Porous anodic aluminium oxide is as a kind of porous nanometer material, and not only the duct is orderly, and the aperture is controlled, and preparation technology's cheap and simple, and it is had broad application prospects in the moisture sensor field, and becomes the study hotspot of recent years.
According to the difference of electrode structure, the moisture sensor take porous anodic aluminium oxide as sensitive material can be divided into parallel-plate structure and coplanar structure.Document (1) Sensors and Actuators B 1998,46,35-41, document (2) Sensors and Actuators B 2000,63,49-54, document (3) Nanotechnology 2009,20,395501 and document (4) Physica E 2010,43,366-371 carries out the segment anode oxidation to aluminium flake, and so that anodised aluminium is not as bottom electrode, anodised aluminium is sensitive layer, be top electrode at anodised aluminium surface deposition gold layer again, obtain the capacitor type moisture sensor of similar sandwich parallel-plate structure.And document (5) Thin Solid Films 2009,517,6198-6210 is at the silicon chip surface deposition of aluminum film of doping high conductivity, by oxidation obtains the anodised aluminium sensitive layer to the aluminium thin film positive pole, then be top electrode at anodised aluminium surface deposition conducting metal palladium layer or gold layer, take the doped silicon matrix of high conductivity as bottom electrode, obtain the capacitor type moisture sensor of similar sandwich parallel-plate structure.Document (6) Sensors and Actuators B 2009,141,441-446 is to the aluminium flake anodic oxidation, obtain the controlled anodic alumina films in aperture, and then anodic alumina films simultaneously deposits the aluminium film of interdigital structure or rectangular coil structure, obtains the capacitor type moisture sensor of coplanar electrode structure.
Above-mentioned document (1), document (2), document (3), document (4) and document (6) are by carrying out anodic oxidation to aluminium flake, obtain the anodised aluminium sensitive layer, this technique and existing microelectronic technique are incompatible, be not suitable for producing in enormous quantities, when particularly document (6) is take anodic alumina films as sensitive layer, consider the fragility of anodised aluminium, more limited its application; Document (5) is by oxidation obtains the anodised aluminium sensitive layer to the aluminium thin film positive pole, this technique and microelectronic technique are compatible, but similar with document (6), top electrode is deposited on the porous anodic aluminium oxide surface, so that the electrode useful area reduces, its sensitivity had impact.
Summary of the invention
Primary and foremost purpose of the present invention is to provide a kind of suitable batch production, avoids reducing the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure of electrode useful area.
For achieving the above object, the present invention has adopted following technical scheme: a kind of electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure comprises insulated substrate, is positioned at a pair of coplanar structure electrode layer on the insulated substrate plate face and is positioned at sensitive layer above coplanar structure electrode layer one end.
Described insulated substrate is glass or quartzy or with the silicon chip of oxide layer; Described a pair of coplanar structure electrode layer has interdigital structure or rectangular coil structure or rectangular configuration, and the coplanar structure electrode layer is the single or multiple lift metallic film; Described sensitive layer is anodic aluminum oxide layer.
The thickness of described anodic aluminum oxide layer is 10～30000 nm, is evenly equipped with the hole that the aperture is 20～400nm on it, and the distribution density in hole is 109/cm
2～1012/cm
2
Described single-layer metal film is tantalum films or titanium film or niobium pentoxide film, and the thickness of single-layer metal film is 10～1000nm; The conductive metal layer that described multiple layer metal film consists of for the first binding layer of being made of tantalum or niobium or titanium, by copper or silver or gold or platinum and the second binding layer that is made of tantalum or niobium or titanium form, the thickness of the first binding layer is 2～1000nm, the thickness of conductive metal layer is 10～1000nm, and the thickness of the second binding layer is 2～1000nm.
Described the second binding layer is positioned on the surface of conductive metal layer one end and is positioned at the below of anodic aluminum oxide layer.
Another object of the present invention is to provide a kind of preparation method of the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure, the method comprises the step of following order:
(1) adopts physical gas-phase deposition and photoetching process, on insulated substrate, prepare first a pair of coplanar structure electrode layer, above coplanar structure electrode layer one end, prepare aluminium lamination again;
(2) aluminium lamination is carried out anodic oxidation, put into again phosphoric acid solution after the oxidation and carry out reaming;
(3) clean oven dry.
Described coplanar structure electrode layer is the single-layer metal film, or be the multiple layer metal film that the first binding layer, conductive metal layer and the second binding layer consist of, when preparation multiple layer metal film, deposit first the first binding layer, then the conductive metal deposition layer deposits the second binding layer on the surface of conductive metal layer one end again; For the multiple layer metal film that contains the second binding layer, the aluminium lamination of deposition covers the second binding layer fully.
When aluminium lamination is carried out anodic oxidation, first the phosphoric acid take concentration as 0.2～1.2 mol/L or oxalic acid or sulfuric acid are 20～200 V as electrolyte at voltage, and temperature is under 0～10 ℃ the condition, aluminium lamination is carried out anodic oxidation, make aluminium lamination become the porous anodic aluminium oxide layer.
Described cleaning, oven dry refer to clean in deionized water, put into baking oven behind the wash clean and dry, and bake out temperature is 100～120 ℃.
Described reaming refers to the porous anodic aluminium oxide layer was immersed in 0.2～10wt% phosphoric acid solution 0～600 minute, makes and is evenly equipped with the aperture that the aperture is 20～400nm on the porous anodic aluminium oxide layer, and its distribution density is 109/cm
2～1012/cm
2
As shown from the above technical solution, the present invention is owing to use physical vapour deposition (PVD) and anode oxidation process, overcome tradition with anodic alumina films during as sensitive material, because anodised aluminium fragility is awkward greatly, cause being difficult to the shortcoming of large-scale application, the preparation method is simple and reliable, and can be compatible with existing micromechanics electronic technology, be suitable for producing in enormous quantities, opened up wide application prospect for this moisture sensor uses.In addition, electrode structure Direct precipitation of the present invention is positioned at anodised aluminium sensitive layer below in insulating body surface, has overcome that electrode has porous structure in the existing electric capacity moisture sensor, the shortcoming that causes useful area to reduce, thus help to improve sensitivity.
Description of drawings
Fig. 1 is structural representation of the present invention;
Fig. 2 is the cut-open view of Fig. 1;
Fig. 3 is the structural representation of a pair of interdigital coplanar structure electrode layer among Fig. 1;
Fig. 4 is the structural representation of a pair of rectangular coil coplanar structure electrode layer among Fig. 1;
Fig. 5 is the structural representation of a pair of rectangle coplanar structure electrode layer among Fig. 1;
Fig. 6 is the capacity measurement curve synoptic diagram that the present invention is tested.
Embodiment
A kind of electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure comprises insulated substrate 1, is positioned at a pair of coplanar structure electrode layer 2 on the insulated substrate 1 plate face and is positioned at sensitive layer 3 above coplanar structure electrode layer 2 one ends.Described insulated substrate 1 is glass or quartzy or with the silicon chip of oxide layer; Described a pair of coplanar structure electrode layer 2 has interdigital structure or rectangular coil structure or rectangular configuration, and coplanar structure electrode layer 2 is the single or multiple lift metallic film; Described sensitive layer 3 is anodic aluminum oxide layer.
The thickness of described anodic aluminum oxide layer is 10～30000 nm, is evenly equipped with the hole that the aperture is 20～400nm on it, and the distribution density in hole is 109/cm
2～1012/cm
2Described single-layer metal film is tantalum films or titanium film or niobium pentoxide film, and the thickness of single-layer metal film is 10～1000nm; The conductive metal layer that described multiple layer metal film consists of for the first binding layer of being made of tantalum or niobium or titanium, by copper or silver or gold or platinum and the second binding layer that is made of tantalum or niobium or titanium form, the thickness of the first binding layer is 2～1000nm, and the thickness of conductive metal layer is 10～1000nm.Described the second binding layer is positioned on the surface of conductive metal layer one end and is positioned at the below of anodic aluminum oxide layer, is comprised of tantalum or titanium or niobium, and the thickness of the second binding layer is 2～1000nm.
This method comprises: (1) adopts physical gas-phase deposition and photoetching process, on insulated substrate 1, prepare first a pair of coplanar structure electrode layer 2, coplanar structure electrode layer 2 is the single-layer metal film, or be the multiple layer metal film that the first binding layer, conductive metal layer and the second binding layer consist of, deposit first the first binding layer for this multiple layer metal film, then the conductive metal deposition layer deposits the second binding layer on the surface of conductive metal layer one end again; Prepare aluminium lamination again above coplanar structure electrode layer 2 one ends, for containing the second binding layer coplanar structure electrode, aluminium lamination covers the second binding layer fully; (2) aluminium lamination is carried out anodic oxidation, put into again phosphoric acid solution after the oxidation and carry out reaming; (3) clean oven dry.
When aluminium lamination is carried out anodic oxidation, first the phosphoric acid take concentration as 0.2～1.2 mol/L or oxalic acid or sulfuric acid are 20～200 V as electrolyte at voltage, and temperature is under 0～10 ℃ the condition, aluminium lamination is carried out anodic oxidation, make aluminium lamination become the porous anodic aluminium oxide layer.Described reaming refers to the porous anodic aluminium oxide layer was immersed in 0.2～10wt% phosphoric acid solution 0～600 minute, makes and is evenly equipped with the aperture that the aperture is 20～400nm on the porous anodic aluminium oxide layer, and its distribution density is 109/cm
2～1012/cm
2Described cleaning, oven dry refer to clean in deionized water, put into baking oven behind the wash clean and dry, and bake out temperature is 100～120 ℃.
Embodiment one
Shown in Fig. 1,2,3,6, elder generation,, dries up with nitrogen after thoroughly cleaning as insulated substrate 1 with quartz, adopts photoetching process and magnetron sputtering, and at a pair of interdigital coplanar structure tantalum layer of insulated substrate 1 deposition, thickness is 200 nm;
Adopt magnetron sputtering, this to interdigital coplanar structure tantalum layer one end above deposit thickness be the aluminium lamination of 1000 nm;
Oxalic acid solution take concentration as 0.3mol/L is electrolyte, be that 3 ℃, anodic oxidation voltage are under the condition of 40V in temperature, above-mentioned multilayer film carried out anodic oxidation, until anodic oxidation is finished, at this moment, aluminium lamination changes the porous anodic aluminium oxide layer that the duct is through hole into;
With the aluminium lamination after the above-mentioned anodic oxidation, with 5 wt% phosphoric acid dip after 30 minutes, place deionized water to clean up after, put into baking oven and dry, bake out temperature is 120 ℃, obtains at last the electric capacity moisture sensor finished product based on the anodic aluminum oxide film coplanar electrode structure.
After testing, the pore size of the porous anodic aluminium oxide layer of this finished product is about 80 nm.
The present embodiment product is carried out capacity measurement, and electric capacity changes with extraneous humidity sees Fig. 6.The having in the different relative humidity atmosphere of saturated solution adjusting that the present embodiment product is placed on different salt carried out in test, and the horizontal ordinate of Fig. 6 is relative humidity, and ordinate is electric capacity.As seen from Figure 6, along with the variation of relative humidity, electric capacity presents larger variation, illustrates that the electric capacity moisture sensor of present embodiment can detect relative humidity variations, has higher sensitivity.
Embodiment two
Shown in Fig. 1,2,4,,, dry up with nitrogen after thoroughly cleaning as insulated substrate 1 with glass, adopt photoetching process and magnetron sputtering, at a pair of rectangular coil coplanar structure titanium layer of insulated substrate 1 deposition, thickness is 150 nm;
Adopt magnetron sputtering, this to rectangular coil coplanar structure tantalum layer one end above deposit thickness be the aluminium lamination of 15000 nm;
Oxalic acid solution take concentration as 0.3mol/L is electrolyte, is that 3 ℃, anodic oxidation voltage are under the condition of 40V in temperature, and above-mentioned multilayer film are carried out anodic oxidation, finishes to the anode oxidation; At this moment, aluminium lamination changes the porous anodic aluminium oxide layer that the duct is through hole into;
With the aluminium lamination after the above-mentioned anodic oxidation, with 5 wt% phosphoric acid dip after 60 minutes, place deionized water to clean up after, put into baking oven and dry, bake out temperature is 120 ℃, obtains at last the electric capacity moisture sensor finished product based on the anodic aluminum oxide film coplanar electrode structure.
After testing, the pore size of the porous anodic aluminium oxide layer of this finished product is about 120 nm.
Embodiment three
Shown in Fig. 1,2,5, with with the silicon chip of silicon dioxide layer as insulated substrate 1, after thoroughly cleaning, dry up with nitrogen, adopt photoetching process and magnetron sputtering, the first binding layer tantalum layer in a pair of rectangle coplanar structure of insulated substrate 1 deposition, then at the first binding layer tantalum layer surface deposition gold layer, at the surface of the surperficial end of gold layer deposition the second binding layer tantalum layer, the first binding layer tantalum layer thickness is 20 nm again, the gold layer thickness is 100 nm, and the second binding layer tantalum layer thickness is 50 nm;
Adopt magnetron sputtering, deposit aluminium lamination above this second binding layer to the rectangular configuration electrode layer, aluminum layer thickness is 1000nm;
Oxalic acid solution take concentration as 0.3mol/L is electrolyte, be that 3 ℃, anodic oxidation voltage are under the condition of 40V in temperature, above-mentioned multilayer film are carried out anodic oxidation, finish to the anode oxidation, at this moment, aluminium lamination changes the porous anodic aluminium oxide layer that the duct is through hole into;
With the aluminium lamination after the above-mentioned anodic oxidation, with 5 wt% phosphoric acid dip after 30 minutes, place deionized water to clean up after, put into baking oven and dry, bake out temperature is 120 ℃, obtains at last the electric capacity moisture sensor finished product based on the anodic aluminum oxide film coplanar electrode structure.
After testing, the pore size of the porous anodic aluminium oxide layer of this finished product is about 80 nm.
In sum, the present invention is owing to use physical vapour deposition (PVD) and anode oxidation process, overcome tradition with anodic alumina films during as sensitive material, because anodised aluminium fragility is awkward greatly, cause being difficult to the shortcoming of large-scale application, the preparation method is simple and reliable, and can be compatible with existing micromechanics electronic technology, be suitable for producing in enormous quantities, opened up wide application prospect for this moisture sensor uses.In addition, electrode structure Direct precipitation of the present invention is positioned at anodised aluminium sensitive layer 3 belows in insulating body surface, has overcome that electrode has porous structure in the existing electric capacity moisture sensor, the shortcoming that causes useful area to reduce, thus help to improve sensitivity.
Claims (10)
1. electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure is characterized in that: comprise insulated substrate, be positioned at a pair of coplanar structure electrode layer on the insulated substrate plate face and be positioned at sensitive layer above coplanar structure electrode layer one end.
2. the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure according to claim 1 is characterized in that: described insulated substrate is glass or quartzy or with the silicon chip of oxide layer; Described a pair of coplanar structure electrode layer has interdigital structure or rectangular coil structure or rectangular configuration, and the coplanar structure electrode layer is the single or multiple lift metallic film; Described sensitive layer is anodic aluminum oxide layer.
3. the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure according to claim 2, it is characterized in that: the thickness of described anodic aluminum oxide layer is 10～30000 nm, be evenly equipped with the hole that the aperture is 20～400nm on it, the distribution density in hole is 109/cm
2～1012/cm
2
4. the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure according to claim 2, it is characterized in that: described single-layer metal film is tantalum films or titanium film or niobium pentoxide film, and the thickness of single-layer metal film is 10～1000nm; The conductive metal layer that described multiple layer metal film consists of for the first binding layer of being made of tantalum or niobium or titanium, by copper or silver or gold or platinum and the second binding layer that is made of tantalum or niobium or titanium form, the thickness of the first binding layer is 2～1000nm, the thickness of conductive metal layer is 10～1000nm, and the thickness of the second binding layer is 2～1000nm.
5. the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure according to claim 4 is characterized in that: described the second binding layer is positioned on the surface of conductive metal layer one end and is positioned at the below of anodic aluminum oxide layer.
6. the preparation method of the described electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure of any one in 5 according to claim 1, the method comprises the step of following order:
(1) adopts physical gas-phase deposition and photoetching process, on insulated substrate, prepare first a pair of coplanar structure electrode layer, above coplanar structure electrode layer one end, prepare aluminium lamination again;
(2) aluminium lamination is carried out anodic oxidation, put into again phosphoric acid solution after the oxidation and carry out reaming;
(3) clean oven dry.
7. the preparation method of the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure according to claim 6, it is characterized in that: described coplanar structure electrode layer is the single-layer metal film, or be the multiple layer metal film that the first binding layer, conductive metal layer and the second binding layer consist of, when preparation multiple layer metal film, deposit first the first binding layer, then the conductive metal deposition layer deposits the second binding layer on the surface of conductive metal layer one end again; For the multiple layer metal film that contains the second binding layer, the aluminium lamination of deposition covers the second binding layer fully.
8. the preparation method of the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure according to claim 6, it is characterized in that: when aluminium lamination is carried out anodic oxidation, phosphoric acid take concentration as 0.2～1.2 mol/L or oxalic acid or sulfuric acid are as electrolyte first, be 20～200 V at voltage, temperature is under 0～10 ℃ the condition, aluminium lamination is carried out anodic oxidation, make aluminium lamination become the porous anodic aluminium oxide layer.
9. the preparation method of the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure according to claim 6, it is characterized in that: described cleaning, oven dry refer to clean in deionized water, put into baking oven behind the wash clean and dry, bake out temperature is 100～120 ℃.
10. the preparation method of the electric capacity moisture sensor based on the anodic aluminum oxide film coplanar electrode structure according to claim 8, it is characterized in that: described reaming refers to the porous anodic aluminium oxide layer was immersed in 0.2～10wt% phosphoric acid solution 0～600 minute, make and be evenly equipped with the aperture that the aperture is 20～400nm on the porous anodic aluminium oxide layer, its distribution density is 109/cm
2～1012/cm
2
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Cited By (2)
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| CN103713022A (en) * | 2013-12-07 | 2014-04-09 | 太原理工大学 | Preparation method for polydimethylsiloxane micro-thin film capacitive biosensor |
| CN104458835A (en) * | 2014-12-26 | 2015-03-25 | 上海集成电路研发中心有限公司 | Humidity sensor and manufacturing method thereof |
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Application publication date: 20130313 |