CN107340325A - A kind of preparation method of the compound field-effect transistor pH sensors of gallium nitride - Google Patents
A kind of preparation method of the compound field-effect transistor pH sensors of gallium nitride Download PDFInfo
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Abstract
A kind of preparation method of the compound field-effect transistor pH sensors of gallium nitride belongs to chemical sensor field, the silicon nano-pillar structure composite that GaN nanometers texture prepared by using plasma chemical gas-phase deposition system is prepared with Ag nano particle Assisted Chemical Etching Process method, pH sensors are made using EGFET forms；By PECVD technique, with simple and green synthesis mode composite gallium nitride (GaN) nanometer texture, composite construction is formed.Compared with Si nano wires, GaN nanometer texture has higher sensitivity, and has bigger surface area, beneficial to the more hydrogen ions of absorption and hydroxide ion.In the range of pH of buffer is 3 to 11, transducer sensitivity increases to 56mV/pH from 38mV/pH.The preparation technology of the present invention is simple and convenient, and the composite construction pH sensors of preparation have preferable performance and good stability.
Description
Technical field：
The invention belongs to chemical sensor field, more particularly, to the EGFET form pH sensors of stable performance and its letter
Just quick preparation technology.
Background technology：
First ion-sensitive field effect transistor (ISFET) of 1970 is used for sensor.It is quick followed by chemistry
Sense film is deposited on the extension grid field effect transistor (EGFET) of the signal thread end of field-effect transistor (FET) gate electrode extension
Start to develop.EGFET has many advantages compared to ISFET, such as high to temperature and the insensitive of light, long-time stability, to material
Material and shape limitation is relatively low, sensing material is not limited to zero defect insulator.
Gallium nitride (GaN) nanometer texture due to specific surface area is higher, carrier mobility is higher and thermodynamics and
The advantages that chemical stability is strong, the extensive concern of researcher is caused.The pH sensor related to GaN also has a lot.
InN/GaN heterojunction structure pH sensors are have studied such as Lee et al., its sensitivity is 52.04mV/pH.Steinhoff et al. is reported
The sensitiveness of road GaN/AlGaN/GaN HEMTs (HEMT) structure is 56.0mV/pH, GaN:Si/GaN:
Mg susceptibilitys are 57.3mV/pH.But most of is using complicated and the HEMT-structure of expensive method preparation, and it is not suitable at present
Commercially produce pH sensors.
Just preparation is being found for this many researcher simply, the excellent preparation technology of stable performance.It is most of at present to grind
Study carefully and concentrate on the development direction of oxide semiconductor pH sensors, but studies have reported that oxide semiconductor is easily with highly basic
Reaction, causes the drift of pH sensor performances, thus find it is a kind of both there is good pH sensitive properties, and can is reached under highly basic
The material for keeping stability is a current resolving ideas.GaN material largely meets above-mentioned requirements, its own
Chemical property it is stable, have fine pH sensitive properties again.Therefore the compound pH sensors of GaN nano materials are developed, are a tools
There is the work of scientific meaning and practical technique value.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the compound field-effect transistor pH sensors of gallium nitride, ensureing
While preferable pH sensitivity, the cost of preparation technology, improving performance stability are reduced.The present invention passes through following technological means
Realize above-mentioned technical purpose:
1st, a kind of preparation method of the EGFET pH chemical sensors of GaN nanometers textural composite silicon nano-pillar, will use etc.
GaN nanometers texture prepared by ion body chemical vapor phase growing (PECVD) system and Ag nano particle Assisted Chemical Etching Process method systems
Standby silicon nano-pillar structure composite, and pH sensors are made using EGFET forms.
2nd, the silicon nanometer rod structure prepared using Ag nano particle Assisted Chemical Etching Process method, is mainly comprised the steps of：
(1) cleaned n-type or p-type silicon chip are placed on to 10-30mL HF (mass fraction 40%) solution and 0.05-
0.10g AgNO3(purity 99.999%) powder and 30-90s in the mixed solution of 50-100mL deionized waters, deposit Ag nanometers
Particle；
(2) silicon chip of the Ag nano particles deposited is then placed on HF (mass fraction 40%), H2O2(mass fraction
30%) and deionized water volume ratio is 20:4:In 76 mixed solution, etching prepares silicon nanometer rod structure, residual metal particles
Removed using concentrated nitric acid；Then use and 5-30nm Au films are deposited under sputter (SBC-12) normal temperature.
3. GaN nanometers texture and the silicon nano-pillar structure composite prepared described in step 2 are prepared using PECVD system, mainly
Comprise the steps of：
(1) GaN nanometers texture prepares and uses PECVD methods, and it is 1 to weigh Ga atoms first with C atomic molars ratio:3-1:12
0.1-0.5g Ga2O3Reaction raw materials are placed on just by the mixed-powder of (purity 99.999%) and activated carbon as reaction raw materials
In beautiful or silica crucible, silicon nano-pillar structural substrates prepared in step 2 are lain in above crucible or side is placed on crucible one
Side, then crucible is put into PECVD tube furnace, heating response, room temperature is naturally cooled to after the completion of reaction, take out sample；
(2) sample surfaces are covered into dustless plastic sheeting, 1- is rolled to a direction using a diameter of 10-50mm steel column
10 times, after the completion of plastic sheeting is removed, obtain a nanometer textural composite structure.
4. making pH sensors using EGFET forms to prepare, mainly comprise the steps of:
(1) wire extraction electrode is fixed into the sample back side prepared in step 3 using conducting resinl, then by the sample back side
Coated completely with insulating cement with sample fixing end with electrode.
5. the conducting resinl described in step 4 includes conductive silver glue, conductive copper glue, conductive carbon paste；Described wire is led comprising copper
Line, paper tinsel wire, aluminum conductor；Described insulating cement includes epoxy resin, silica gel, rosin paraffin.
Beneficial effects of the present invention：
1. the preparation technology of the present invention is simple and convenient, the composite construction pH sensors of preparation have preferable performance and well
Stability.In the range of pH of buffer is 3 to 11, transducer sensitivity increases to 56mV/pH from 38mV/pH.
2. preparation method is simple, green, suitable for the large-scale production of commercial applications.
3. preparing parameter used by composite construction, it can ensure that it obtains suitable composite construction so as to obtain in the range of
To optimal effect:In parameter area nano-pillar can be made to obtain suitable length used by preparation Si nano-pillars, be unlikely to
It is too short or it is oversize make nano-pillar bending can all influence sensing capabilities；Preparing used by GaN nanometer texture in parameter area can be with
Make GaN nanometer texture obtain suitable length be unlikely to it is oversize make texture too it is close lack hole or too short-bore gap too it is big influence sensing
Performance, the density for obtaining suitable nanometer texture are to obtain the essential condition of optimal sensing capabilities.
Brief description of the drawings
Fig. 1 embodiment 1Si nanometer rod structure SEM pictures
Fig. 2 embodiment 2Si and GaN nanometer textural composite structure SEM pictures
Fig. 3 embodiment 3Si and GaN nanometer textural composite structure SEM pictures
Fig. 4 embodiments 1 and EGFET form pH sensor test schematic diagrames in embodiment 2
Fig. 5 embodiment 1Si nanometer rod structures prepare sensor and responded in the solution that pH value is 3 to 11
Fig. 6 embodiment 1Si nanometers rod structure prepares transducer sensitivity curve
Fig. 7 embodiment 2Si and GaN nanometer textural composite structures prepare sensor and responded in the solution that pH value is 3 to 11
Fig. 8 embodiment 2Si and GaN nanometer textural composites structure prepares transducer sensitivity curve
Fig. 9 embodiment 3Si and GaN nanometer textural composite structures prepare sensor and responded in the solution that pH value is 3 to 11
Figure 10 embodiment 3Si and GaN nanometer textural composites structure prepares transducer sensitivity curve
Embodiment
Present invention side uses new composite structural design, realizes the test of pH performances high sensitivity and high stability, and
And Making programme is simple, quick, cost is relatively low, so as to greatly improve practicality.
Embodiment 1
(1) 0.085g AgNO are weighed3Powder is dissolved in 80mL deionized waters, and 20mL HF acid is added dropwise and prepares solution, will
The silicon chip of the n-type low-resistance silicon (resistivity 0.001-0.009 Ω cm) cleaned up is put into above-mentioned solution after immersion 60s taking-ups
5s cleanings surface is soaked in deionized water, is subsequently dipped to HF (mass fraction 40%):H2O2(mass fraction 30%):H2O volumes
Than for 20:4:30min is etched in 76 mixed solution, the silicon chip extracting completed will be reacted in concentrated nitric acid (mass fraction 68%)
Immersion 2h removes unnecessary Ag, then using a large amount of deionized water rinsings.Then use and deposited under sputter (SBC-12) normal temperature
20nm Au。
(2) copper cash extraction electrode is fixed into the above-mentioned sample back side prepared using copper conductive adhesive, then using asphalt mixtures modified by epoxy resin
Fat glue coats at the sample back side and electrode with sample fixing end completely.
Embodiment 2
(1) 0.085g AgNO are weighed3Powder is dissolved in 80mL deionized waters, and 20mL HF acid is added dropwise and prepares solution, will
The silicon chip of the n-type low-resistance silicon (resistivity 0.001-0.009 Ω cm) cleaned up is put into above-mentioned solution after immersion 60s taking-ups
5s cleanings surface is soaked in deionized water, is subsequently dipped to HF (mass fraction 40%):H2O2(mass fraction 30%):H2O volumes
Than for 20:4:30min is etched in 76 mixed solution, the silicon chip extracting completed will be reacted in concentrated nitric acid (mass fraction 68%)
Immersion 2h removes unnecessary Ag, then using a large amount of deionized water rinsings.Then using using under sputter (SBC-12) normal temperature
Deposit 20nm Au.
(2) GaN nanometers texture prepares and uses PECVD methods, weighs mol ratio first as 1：12(Ga:C 0.3g's)
Ga2O3(purity 99.999%), as reaction raw materials, reaction raw materials is placed on inside silica crucible, incited somebody to action with activated carbon mixed-powder
The substrate side prepared in above-mentioned steps (1) is placed on crucible side, is then pushed into crucible in PECVD tube furnace, specific reaction
Parameter is：Back end vacuum 1Pa, 20sccm N2, 10sccm H2, 880 DEG C of reaction temperature.Radio-frequency power 80W, reaction pressure 45Pa,
Reaction time 30min.Room temperature is naturally cooled to after the completion of reaction, takes out sample.
(3) sample surfaces are covered into dustless plastic sheeting, rolled 5 times to a direction using a diameter of 10mm rod iron,
After the completion of plastic sheeting is removed, obtain a nanometer textural composite structure.
(4) copper cash extraction electrode is fixed into the above-mentioned sample back side prepared using copper conductive adhesive, then using asphalt mixtures modified by epoxy resin
Fat glue coats at the sample back side and electrode with sample fixing end completely.
Embodiment 3
(1) 0.065g AgNO are weighed3Powder is dissolved in 60mL deionized waters, and 10mL HF acid is added dropwise and prepares solution, will
The silicon chip of the p-type low-resistance silicon (resistivity 0.001-0.009 Ω cm) cleaned up is put into above-mentioned solution after immersion 60s taking-ups
5s cleanings surface is soaked in deionized water, is subsequently dipped to HF (mass fraction 40%):H2O2(mass fraction 30%):H2O volumes
Than for 20:4:20min is etched in 76 mixed solution, the silicon chip extracting completed will be reacted in concentrated nitric acid (mass fraction 68%)
Immersion 1.5h removes unnecessary Ag, then using a large amount of deionized water rinsings.Then use sputter (SBC-12) normal temperature
Lower deposition 10nm Au.
(2) GaN nanometers texture prepares and uses PECVD methods, weighs mol ratio first as 1：6(Ga:C the Ga of 0.2g)2O3
Reaction raw materials are placed on inside silica crucible as reaction raw materials by (purity 99.999%) and activated carbon mixed-powder, will be above-mentioned
The substrate side prepared in step (1) is placed on crucible side, is then pushed into crucible in PECVD tube furnace, specific response parameter
For：Back end vacuum 1Pa, 20sccm N2, 10sccm H2, 880 DEG C of reaction temperature.Radio-frequency power 80W, reaction pressure 45Pa, reaction
Time 30min.Room temperature is naturally cooled to after the completion of reaction, takes out sample.
(3) sample surfaces are covered into dustless plastic sheeting, rolled 10 times to a direction using a diameter of 10mm rod iron,
After the completion of plastic sheeting is removed, obtain a nanometer textural composite structure.
(4) aluminum steel extraction electrode is fixed into using silver conductive adhesive in the above-mentioned sample back side prepared, then uses rosin stone
Wax coats at the sample back side and electrode with sample fixing end completely.
Claims (3)
- A kind of 1. preparation method of the compound field-effect transistor pH sensors of gallium nitride, by using plasma chemical vapor deposition The silicon nano-pillar structure composite that GaN nanometers texture prepared by system is prepared with Ag nano particle Assisted Chemical Etching Process method, use EGFET forms make pH sensors；The silicon nanometer rod structure of preparation, is comprised the steps of：(1) cleaned silicon chip is placed on to HF (solution and the 0.05-0.10g AgNO of 10-30mL mass fraction 40%3Powder With 30-90s in the mixed solution of 50-100mL deionized waters, Ag nano particles are deposited；(2) silicon chip of the Ag nano particles deposited is then placed on the HF solution of mass fraction 40%, mass fraction 30% H2O2In solution and the mixed solution that deionized water volume ratio is 20: 4: 76, etching 10-60min prepares silicon nanometer rod structure, residual Remaining metallic particles soaks 10-180min removals in concentrated nitric acid；Then use and 5-30nm Au films are deposited under sputter normal temperature；GaN nanometers texture and prepared silicon nano-pillar structure composite will be prepared using PECVD system, comprised the steps of：(1) GaN nanometers texture prepares and uses PECVD methods, weighs Ga atoms and C atomic molars ratio as 1: 3-1: 12 0.1- 0.5g Ga2O3Reaction raw materials are placed in corundum or silica crucible as reaction raw materials by the mixed-powder of powder and activated carbon, Prepared silicon nano-pillar structural substrates are lain in above crucible or side is placed on crucible side, crucible is then put into PECVD Tube furnace in, heating response, specific response parameter is：Back end vacuum 1Pa, 20sccmN2, 10sccm H2, reaction temperature 880 ℃；Radio-frequency power 80W, reaction pressure 45Pa, reaction time 30min；Room temperature is naturally cooled to after the completion of reaction, takes out sample；(2) sample surfaces are covered into dustless plastic sheeting, 1-10 is rolled to a direction using a diameter of 10-50mm steel column It is secondary, after the completion of plastic sheeting is removed, obtain a nanometer textural composite structure.
- 2. a kind of preparation method of the compound field-effect transistor pH sensors of gallium nitride according to claim 1, its feature It is, making pH sensors using EGFET forms prepares, and comprises the steps of:The nanometer textural composite structured rear surface prepared is fixed into wire extraction electrode using conducting resinl, then by the sample back side and Electrode and sample fixing end cladding completely.
- 3. a kind of preparation method of the compound field-effect transistor pH sensors of gallium nitride according to claim 2, its feature It is, described conducting resinl includes conductive silver glue, conductive copper glue, conductive carbon paste；Described wire include copper conductor, paper tinsel wire, Aluminum conductor；Described insulating cement includes epoxy resin, silica gel, rosin paraffin.
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Cited By (4)
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| CN108548864A (en) * | 2018-03-20 | 2018-09-18 | 上海交通大学 | Plasma gas sensor and its manufacturing method |
| CN112525954A (en) * | 2020-12-02 | 2021-03-19 | 西安交通大学 | Preparation method of porous gallium nitride-based room temperature gas sensor |
| CN113930745A (en) * | 2021-09-30 | 2022-01-14 | 北京工业大学 | Preparation method of high-crystallization GaN film |
| CN116754617A (en) * | 2023-08-17 | 2023-09-15 | 太原理工大学 | GaN-Metal/PANI ammonia sensor and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108548864A (en) * | 2018-03-20 | 2018-09-18 | 上海交通大学 | Plasma gas sensor and its manufacturing method |
| CN112525954A (en) * | 2020-12-02 | 2021-03-19 | 西安交通大学 | Preparation method of porous gallium nitride-based room temperature gas sensor |
| CN113930745A (en) * | 2021-09-30 | 2022-01-14 | 北京工业大学 | Preparation method of high-crystallization GaN film |
| CN116754617A (en) * | 2023-08-17 | 2023-09-15 | 太原理工大学 | GaN-Metal/PANI ammonia sensor and preparation method and application thereof |
| CN116754617B (en) * | 2023-08-17 | 2023-10-27 | 太原理工大学 | GaN-Metal/PANI ammonia sensor and preparation method and application thereof |
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