CN106644982A - Method for preparing pyroelectric spectrum detector of gas analyzer - Google Patents
Method for preparing pyroelectric spectrum detector of gas analyzer Download PDFInfo
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- CN106644982A CN106644982A CN201611219544.2A CN201611219544A CN106644982A CN 106644982 A CN106644982 A CN 106644982A CN 201611219544 A CN201611219544 A CN 201611219544A CN 106644982 A CN106644982 A CN 106644982A
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- film
- platinum
- spectrum detector
- gas analyzer
- pyroelectric
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The invention discloses a method for preparing a pyroelectric spectrum detector of a gas analyzer. The method comprises seven preparation steps. According to the method, an inorganic-organic hybrid porous SiO2 thin film material is adopted as a heat insulation structure, so that the problems of weak mechanical strength, high cracking, collapse and separation rate and the like of an integrated device heat insulation structure which adopts a microbridge structure, a suspended structure and an air gap structure at present are solved, and the mechanical performance and impact resistance of an integrated pyroelectric spectrum detector chip are improved.
Description
Technical field
The invention belongs to photoelectricity and micro-electromechanical system field, are specifically related to a kind of gas analyzer pyroelectricity spectrum
The preparation method of detector.
Background technology
Because most toxic and harmfuls all have certain absorption to the spectrum of a certain wave band, so according to this
The principle of absorption of spectrum can be achieved with the preparation of toxic and harmful analyzer.In general, toxic and harmful is to a certain ripple
The absorption of the spectrum of section coincide than ear-Lambert law：
P=P0Exp(-kcl)
Wherein P0Energy P produced by light source be by there is under test gas environment after remaining energy, k is to absorb
Coefficient, l is distance of the light source away from detector cells, and c is under test gas concentration.
In actual applications, the light radiation for being sent by light source is converted into voltage signal, sensor on by spectrum sensor
Voltage output affected by GAS ABSORPTION in air chamber and changed, gas concentration is higher, and absorbed light is higher, on sensor
Output voltage is lower, and gas concentration is lower, and the light of absorption is fewer, and the voltage of sensor output is higher.The voltage of sensor output
It is premenstrual to put after amplifier, difference amplifier amplification, calculated into one-chip computer or DSP, according to
Mathematical Modeling and there is related parameter to calculate concentration.
Spectrum sensor is the core electron components and parts of toxic and harmful analyzer, and its performance parameter is directly influenced
The performance of gas analyzer such as detection sensitivity.Spectral energy receiving device used by alternative gas analyzer has thermoelectricity
Heap-type detector, thermosensitive resistance type detector and pyroelectric detector three major types.Thermocouple type detector voltage response signal compared with
It is little, and temperature noise is too big, and thermosensitive resistance type detector temperature noise is too big, it is extremely difficult to correct.So pyroelectric detector is
Using main flow.
The difference of the form of the photoelectric functional material adopted according to spectrum sensor device, the technology of pyroelectric sensor
Route have two it is available：One hybrid devices processing technology routine for being to adopt ceramic material or crystalline material, separately
One is using the integrated form device technology technology path of thin-film material.The preparation of hybrid devices is needed first photosensitive first material
(ferroelectric ceramics) thinning, grinding, is deposited with upper/lower electrode again after polishing, completes welding encapsulation again therewith, and its technique is complex, special
It is not that on material reduction process, thus yield rate is very inexpensive higher, so-called device is worked it out.Integrated form device then may be used
With the growth for once just completing heat insulator, bottom electrode, ferroelectric thin film and Top electrode on one piece of substrate, subsequent technique is such as
Scribing, welding and encapsulation etc. are just as ceramic-type.Its advantage is that technique is relatively simple, core technology break through after yield rate
Can be very high (thousand of unit components can be grown in one piece of 5 inch plaques, so-called device is longer).
At present the major part used by the spectral energy receiving device used by all kinds of toxic and harmful analyzers is hybrid
Pyroelectric electric device, its shortcoming has following three aspect：First, hybrid pyroelectric electric device operating frequency is relatively low, can only be in low frequency
Section such as 0.1Hz-5Hz frequency bands work could meet higher voltage responsive signal, and in this low-frequency range such as 0.1Hz-5Hz frequencies
Rate section, outside noise is very big such as white noise；2nd, hybrid pyroelectric electric device is affected larger by environmental temperature fluctuation, is needed accurate
Temperature correction；3rd, the impact of hybrid pyroelectric electric device vibrated (such as wind) is larger, brings larger noise signal, affects
Zero point is stablized.
And integrated form pyroelectric electric device can overcome as above shortcoming for hybrid pyroelectric electric device：First, integrated form
Pyroelectric electric device operating frequency is higher, also can meet higher voltage responsive in high band such as 10Hz-200Hz frequency bands work
Signal, and in this frequency range, low frequency white noise is avoided, meet ppm level gas concentration detection sensitivities；2nd, integrated thermal is released
The impact of electrical part vibrated (such as wind) is less big, and the noise signal brought is little, has substantially no effect on stablizing for zero point.
Therefore, hybrid pyroelectric electric device is replaced as the spectrum energy used by gas analyzer using integrated form pyroelectric electric device
Amount receiving device will greatly improve the signal to noise ratio of system, and then improve detection sensitivity.
The content of the invention
It is an object of the invention to provide a kind of preparation method of gas analyzer pyroelectric spectrum detector, solves current
Hybrid pyroelectric infrared detector exist can only the external environments such as low-frequency range work, vibrated and wind change impact compared with
Greatly, the system signal noise ratio that brought is poor thus in the spectral energy receiving device for gas analyzer, detection sensitivity
Relatively low shortcoming.
To achieve these goals, a kind of gas analyzer pyroelectric spectrum detector of offer is provided
Preparation method, its step is as follows：
Step one：Based on monocrystalline silicon, surface prepares porous SiO of inorganic-organic hybridization2Film is thermal insulation structure
Film；
Step 2：Using direct current magnetron sputtering process inorganic-organic hybridization porous SiO2Platinum/titanium is prepared on film
Film is lower electrode film and is completed graphically using positive glue stripping method, depending on its size dimension is according to design requirement；
Step 3：Optoelectronic film is prepared simultaneously on platinum/platinum/titanium metal thin film using radio-frequency magnetron sputter method or sol-gal process
Completed graphically using dry and wet etch, depending on its size dimension is according to design requirement；
Step 4：Upper electrode film is prepared on optoelectronic film using direct current magnetron sputtering process or Vacuum sublimation and is adopted
Completed graphically with dry and wet etch, depending on its size dimension is according to design requirement；
Step 5：One layer of chip protection layer is grown on upper electrode film using plasma-reinforced chemical sedimentation, and is pressed
Design requirement completes scribing.
Step 6：Prepare the signal processing circuit converted based on impedance according to a conventional method by design requirement, and complete chip
Bonding and lead welding between signal processing circuit board.
Step 7：Chip and signal processing circuit board are packaged in into the shell with infrared window and base by design requirement
In, that is, complete the making of integrated form pyroelectric spectrum detector.
In step 2, the thickness of the platinum/platinum/titanium metal thin film is 50nm-100nm.
In step 3, the optoelectronic film is PZT (lead zirconate titanate) series or BST (barium strontium titanate) series ferroelectric thins
Film, the thickness of the optoelectronic film is 400nm-1000nm.
In step 4, the upper electrode film is chromium/thin nickel metal film, and the upper electrode film square resistance is 300
Ω-1000Ω。
In step 5, the chip protection layer is silicon nitride film, and the thickness of the silicon nitride film is 200nm-
500nm。
The advantages of the present invention are：
1st, the method that the present invention is provided replaces ferro-electricity single crystal or ferroelectric ceramic material electrically susceptible as light using ferroelectric thin-flim materials
Sense material, replaces hybrid combination to prepare pyroelectric spectrum detector with integrated structure, enables the operating frequency of device
Increase substantially, from 0.1Hz-5Hz frequency bands 10Hz-100Hz frequency bands are brought up to, avoid low frequency white noise, examine system
Survey sensitivity to be improved.
2nd, the method that the present invention is provided replaces ferro-electricity single crystal or ferroelectric ceramic material electrically susceptible as light using ferroelectric thin-flim materials
Sense material, replaces hybrid combination to prepare pyroelectric infrared detector, in the light for gas analyzer with integrated structure
The impact of vibrated (such as wind) and ambient temperature change is less during spectrum energy receiving device, and the noise signal brought is little, makes system
Detection sensitivity is improved, and does not affect stablizing for zero point.
3rd, the method that the present invention is provided adopts porous SiO of inorganic-organic hybridization2Thin-film material as thermal insulation structure,
Overcome and adopt at present micro-bridge structure, hanging structure and air-gap structure as the machine of the presence of integrated form device thermal insulation structure
Tool intensity difference, the problems such as be susceptible to be cracked, cave in, come off, improve integrated thermal and release the mechanics that electric light composes detector chip
Performance and shock resistance.
Description of the drawings
Fig. 1 is that the structural representation of the preparation method of gas analyzer pyroelectric spectrum detector of the present invention is intended to；
In accompanying drawing, the list of parts representated by each label is as follows：
1- silicon single crystal；2- thermal insulation structure films；3- lower electrode films；4- optoelectronic films；5- upper electrode films；6- chips
Protective layer.
Specific embodiment
The specific embodiment of the present invention is further described with reference to the accompanying drawings and examples, following examples are only used
In clearly illustrating technical scheme, and can not be limited the scope of the invention with this.
The technical scheme that the present invention is embodied as is：
Step one：Based on monocrystalline silicon, surface prepares porous SiO of inorganic-organic hybridization2Film is thermal insulation structure
Film；
With crystal orientation as (100) direction, body resistivity be 0.1-10 Ω cm, size dimension as 20cm × surface of 20cm
Based on the monocrystalline silicon of thermal oxide, porous SiO of the inorganic-organic hybridization that thickness is 1um-5um is prepared2Film；
Step 2：Using direct current magnetron sputtering process inorganic-organic hybridization porous SiO2Platinum/titanium is prepared on film
Film is lower electrode film and is completed graphically using positive glue stripping method, depending on its size dimension is according to design requirement；
By the porous-SiO of inorganic-organic hybridization of the structural parameters of designed device obtained by step one2Film
On complete after photoetching process, platinum/platinum/titanium metal thin film is prepared using direct current magnetron sputtering process and figure is completed using positive glue stripping method
Change, be described as follows：
1st, the structural parameters of the device involved by photoetching process are expressed as follows：
(1) photosensitive first number：It is polynary that unit, 2 × 1-128 × 1 short-term arrange polynary, 2 × 2-9 × 9 partial array；
(2) photosensitive first size dimension：ф1mm-ф3、1mm×1mm-3mm×3mm；
(3) photosensitive first spacing：0.2mm-3mm.
2nd, the structural parameters of the platinum/platinum/titanium metal thin film involved by the photoetching process of positive glue stripping method are expressed as follows：
(4) press welding block size dimension：ф0.5mm-ф3、0.5mm×0.5mm-3mm×3mm；
(5) wire widths：0.2mm-1mm；
3rd, the process goal of positive glue stripping method is exactly porous SiO in thickness for the inorganic-organic hybridization of 1um-5um2It is thin
Prepare the platinum titanium metal film of its figure in film substrate, the direct current magnetron sputtering process growth technique of involved platinum titanium metal film
Parameter is：
| Working gas | Target-substrate distance | Operating pressure | Sputtering power | Sputtering time |
| Argon gas | 70mm | 2.6Pa | 79w | Platinum 15s, titanium 8s |
The thickness of metallic film is 50nm-100nm, and the size dimension of metallic film has increased than photosensitive first size dimension
Plus, but its increasing degree is with 1/4 being advisable less than photosensitive first spacing；
Step 3：Optoelectronic film is prepared simultaneously on platinum/platinum/titanium metal thin film using radio-frequency magnetron sputter method or sol-gal process
Completed graphically using dry and wet etch, depending on its size dimension is according to design requirement；
1st, using radio-frequency magnetron sputter method it is obtained by step 2, completed on patterned platinum/platinum/titanium metal thin film prepare
BST(Ba0.65Sr0.35TiO3Barium strontium titanate) used as optoelectronic film, the thickness of optoelectronic film is 400nm～1000nm to ferroelectric thin film.
Its growthing process parameter is：
| Sputtering power | Substrate temperature | Sputtering pressure | Oxygen Ar Pressure | Target-substrate distance | Automatic bias |
| 150w | 550℃ | 5Pa | 1:9 | 50mm | 115v |
2nd, photoetching process is completed using positive glue, and BST optoelectronic films is completed graphically using wet etch, optoelectronic film
Cell size size should increased than photosensitive first size dimension, but its increasing degree is advisable with the 1/4-1/2 of photosensitive first spacing.
Its wet etch technological parameter be：
(1) wet etching corrosion agent prescription is HF：HNO3：H2O=2：10：100；
(2) the wet etching time：- 20 seconds 10 seconds；
Step 4：Upper electrode film is prepared on optoelectronic film using direct current magnetron sputtering process or Vacuum sublimation and is adopted
Completed graphically with dry and wet etch, depending on its size dimension is according to design requirement；
1st, to complete patterned BST optoelectronic films as substrate obtained by step 3, using direct current magnetron sputtering process
Chromium/thin nickel metal film is prepared as Top electrode, the square resistance of chromium/nickel film is 300 Ω -1000 Ω, involved chromium/nickel gold
Category film direct current magnetron sputtering process growthing process parameter be：
| Working gas | Target-substrate distance | Operating pressure | Sputtering power | Sputtering time |
| Argon gas | 70mm | 2.2Pa | 75w | Nickel 30s, chromium 60s |
2nd, photoetching process is completed using positive glue, and chromium/nickel is completed using wet etching method Film patterning, chromium/nickel film
Feature size size is than photosensitive first size dimension；
Step 5：One layer of chip protection layer is grown on upper electrode film using plasma-reinforced chemical sedimentation, and is pressed
Design requirement completes scribing；
1st, it is working gas in the chip obtained by step 4 with silane and ammonia using plasma-reinforced chemical sedimentation
Upper grown silicon nitride film, its thickness is about 300nm, and the technological parameter of involved plasma-reinforced chemical sedimentation is：Deng
Ion strengthens chemical deposition (PECVD) grown silicon nitride thin-film technique condition
| Carrier gas | Power | Working gas 1 | Working gas 2 | Growth time |
| Argon gas | 280w | Silane SiH4 | Ammonia NH3 | 1.5 hours |
2nd, the feature size of silicon nitride film deducts again pressure for the feature size of the platinum/platinum/titanium metal thin film described in second step
The size of welding block, the removal technique of the silicon nitride film in the patterning process of silicon nitride film sends out etching method (reaction using dry
Ion etching method), its process conditions following table：Reactive ion etching method removes carborundum films process conditions
| Carrier gas | Power | Reacting gas | Etch period |
| Argon gas | 250w | Sulfur hexafluoride SF6 | 1.2 hours |
Step 6：Prepare the signal processing circuit converted based on impedance according to a conventional method by design requirement, and complete chip
Bonding and lead welding between signal processing circuit board；
Step 7：Chip and signal processing circuit board are packaged in into the shell with infrared window and base by design requirement
In, that is, complete the making of integrated form pyroelectric spectrum detector.
Scribing is carried out to the multiple material chips made by above-mentioned steps, the material chip after scribing and process circuit are connected
Connect and be packaged, that is, complete the making of multiple integrated form pyroelectric infrared detectors.
1st, using scribing machine, knife completes scribing under the intersection of each material chip, from the silicon chip of full wafer 20mm × 20mm
On obtain same more sheets chip, and complete some material chip press welding block and wherein between one end of chip link
Welding.
2nd, chip and signal processing circuit board are bonded together, and complete the other end of chip link with and signal at
The welding of reason circuit board leads, obtains material chip component.
3rd, the shell encapsulation of material chip component, band wherein spectral window and base is completed shown in multiple this method
A kind of integrated form pyroelectric infrared detector making.Wherein spectral window is narrow band pass filter, and its centre wavelength is
For the absorbing wavelength of the infrared spectrum of under test gas.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, on the premise of without departing from the technology of the present invention principle, some improvements and modifications can also be made, these improvements and modifications
Also should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of gas analyzer pyroelectric spectrum detector, its step is as follows：
Step one：Based on monocrystalline silicon, surface prepares porous SiO of inorganic-organic hybridization2Film is thermal insulation structure film；
Step 2：Using direct current magnetron sputtering process inorganic-organic hybridization porous SiO2Platinum/platinum/titanium metal thin film is prepared on film
Complete graphically for lower electrode film and using positive glue stripping method, depending on its size dimension is according to design requirement；
Step 3：Optoelectronic film is prepared on platinum/platinum/titanium metal thin film using radio-frequency magnetron sputter method or sol-gal process and is adopted
It is dry to send out and wet etch is completed graphically, depending on its size dimension is according to design requirement；
Step 4：Upper electrode film is prepared and using dry on optoelectronic film using direct current magnetron sputtering process or Vacuum sublimation
Send out and wet etch is completed graphically, depending on its size dimension is according to design requirement；
Step 5：One layer of chip protection layer is grown on upper electrode film using plasma-reinforced chemical sedimentation, and by design
Requirement completes scribing；
Step 6：Prepare the signal processing circuit converted based on impedance according to a conventional method by design requirement, and complete chip with letter
Bonding and lead welding between number process circuit plate；
Step 7：In the shell with infrared window and base, i.e., chip and signal processing circuit board are packaged in by design requirement
Complete the making of integrated form pyroelectric spectrum detector.
2. a kind of preparation method of gas analyzer pyroelectric spectrum detector as claimed in claim 1, it is characterised in that：
In step 2, the thickness of the platinum/platinum/titanium metal thin film is 50nm-100nm.
3. a kind of preparation method of gas analyzer pyroelectric spectrum detector as claimed in claim 1, it is characterised in that：
In step 3, the optoelectronic film is PZT (lead zirconate titanate) series or BST (barium strontium titanate) series ferroelectric thin films, the photoelectricity
The thickness of film is 400nm-1000nm.
4. a kind of preparation method of gas analyzer pyroelectric spectrum detector as claimed in claim 1, it is characterised in that：
In step 4, the upper electrode film is chromium/thin nickel metal film, and the upper electrode film square resistance is 300 Ω -1000 Ω.
5. a kind of preparation method of gas analyzer pyroelectric spectrum detector as claimed in claim 1, it is characterised in that：
In step 5, the chip protection layer is silicon nitride film, and the thickness of the silicon nitride film is 200nm-500nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611219544.2A CN106644982A (en) | 2016-12-26 | 2016-12-26 | Method for preparing pyroelectric spectrum detector of gas analyzer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611219544.2A CN106644982A (en) | 2016-12-26 | 2016-12-26 | Method for preparing pyroelectric spectrum detector of gas analyzer |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102721658A (en) * | 2012-07-05 | 2012-10-10 | 昆明斯派特光谱科技有限责任公司 | Method for manufacturing pyroelectric spectrum detector |
| CN202502046U (en) * | 2012-03-06 | 2012-10-24 | 昆明斯派特光谱科技有限责任公司 | Light spectrum transmitting terminal for spectroscopy gas analyzer |
| CN105973831A (en) * | 2016-06-30 | 2016-09-28 | 电子科技大学 | Four-path gas component measurement pyroelectric infrared detector |
-
2016
- 2016-12-26 CN CN201611219544.2A patent/CN106644982A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202502046U (en) * | 2012-03-06 | 2012-10-24 | 昆明斯派特光谱科技有限责任公司 | Light spectrum transmitting terminal for spectroscopy gas analyzer |
| CN102721658A (en) * | 2012-07-05 | 2012-10-10 | 昆明斯派特光谱科技有限责任公司 | Method for manufacturing pyroelectric spectrum detector |
| CN105973831A (en) * | 2016-06-30 | 2016-09-28 | 电子科技大学 | Four-path gas component measurement pyroelectric infrared detector |
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Application publication date: 20170510 |