CN107188184A - The hydrothermal preparing process of porous silica material and the preparation method of gas fluorescent optical sensor - Google Patents
The hydrothermal preparing process of porous silica material and the preparation method of gas fluorescent optical sensor Download PDFInfo
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- CN107188184A CN107188184A CN201710293877.8A CN201710293877A CN107188184A CN 107188184 A CN107188184 A CN 107188184A CN 201710293877 A CN201710293877 A CN 201710293877A CN 107188184 A CN107188184 A CN 107188184A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
It is used for explosive fluoroscopic examination material preparation method, more particularly to a kind of hydrothermal preparing process of porous silica material the present invention relates to one kind, the hydrothermal preparing process of porous silica material comprises the following steps：Monocrystalline silicon piece is fixed in the liner of hydrothermal reaction kettle after over cleaning, injects etchant solution within the liner, and etchant solution is the HF solution of mass fraction 30% 50% and the 1mol/L of concentration 0.3 zinc nitrate solution, and the volume ratio of HF solution and zinc nitrate solution is 2.5:1‑6:1；Liner is put in hydrothermal reaction kettle shell, hydrothermal reaction kettle is placed in baking oven and carries out heating response, question response terminates to be cooled to after room temperature, monocrystalline silicon piece is taken out and rinses well, drying is taken out after hydrogen peroxide dipping；The present invention has the advantages that high porosity, luminous intensity height, surface apertures are homogeneous as a result of above technical scheme, the porous silica material of preparation；The porous silicon prepared using technical solution of the present invention has fluorescence intensity high as the gas fluorescent optical sensor of substrate, and film forming is homogeneous, reference area is high, excellent adsorption the advantages of.
Description
Technical field
Hydro-thermal the present invention relates to one kind for explosive fluoroscopic examination material preparation method, more particularly to porous silica material
The preparation method of preparation method and gas fluorescent optical sensor.
Background technology
As the attack of terrorism is more and more fiery, terrorist activity seriously threatened social safety, people's property safety, life
Safety etc., therefore, if we can effectively detect explosive, it will to society, the life security and property safety of the people
Bigger guarantee is provided.The various technologies such as police dog, ion mobility spectrometry, x-ray imaging, mass spectrum all apply to detect explosive, but
It is that police dog is due to its work fatigue, and instrument is existed again to be had the shortcomings that radioactive source, volume are big and limit it in real life
In use.It is emerging technology that harmful influence is detected by fluorescence quenching method, and it is without radioactive source, small volume, spirit
The advantages of sensitivity is high attracts increasing researcher.At present, the explosive detection technology by principle of fluorescent quenching is being just
In continue to develop improve during, its highly sensitive gas fluorescent optical sensor mainly has following several：1st, unimolecule is passed through
Different fluorescent small molecules and different length, the linking arm of structure are grown on tabular quartz glass by self assembly, so as to obtain
Studies of Fluorescent Film Sensors.2nd, fluorescence molecule is prepared into solution, obtained by the siphonage of capillary quartz glass tube with hair
Fine quartz glass tube is the Studies of Fluorescent Film Sensors that substrate inwall has fluorescence molecule.
Above-mentioned fluorescent optical sensor all uses quartz glass as substrate, and quartz substrate surface does not all have porous knot
Structure, simply simply make use of its smooth surface, for loose structure, the small adsorptivity of its specific surface area is poor.Porous silicon
Be one kind using nanometer silicon atom as skeleton, structure is loose spongiform semi-conducting material, with specific surface area it is big (>500m2/
Cm3), the outstanding advantage such as luminescence generated by light.Therefore, the fluorescent optical sensor and above-mentioned fluorescence being prepared from using porous silicon as substrate
Sensor is compared, convenient with preparing, simple to operate, and sensitivity is high, prepare low cost and other advantages.
Anodic attack method is the most common method for preparing porous silicon, and using silicon chip as anode, platinum electrode is used as negative electrode, HF
Electrochemical corrosion is carried out as electrolyte.People's solution ratio different by adjusting, different corrosion currents, different corrosion
Time and the porous silicon that different pore size is obtained using different types of silicon chip, and aperture can be from micropore to mesoporous to big
Hole is adjustable.But this method has the following disadvantages：1. the porous silicon of generation is more easily damaged.2. silicon chip is easy in corrosion process
It is destroyed.3. poor repeatability.However, hydro-thermal method solves these problems well.
At present, the method preparation process that a kind of hydro-thermal method excessively that Chinese University of Science and Technology announces prepares porous silicon is as follows：1.p type silicon chips
(resistivity is 0.005 Ω .cm-1) is positioned in polytetrafluoroethyllining lining.2. in a reservoir add 0.2mol/LLiF and
4.0mol/LHNO3 mixed solutions, filling rate is 70%.3. liner is put into rustless steel container, baking oven is transferred to, 160 degree,
6H.Obtain that surface apertures are homogeneous, stable luminescence porous silicon by this method, but there is showing for blue shift in the porous silicon prepared
As, and luminous intensity is inadequate.
The content of the invention
There is the phenomenon of blue shift for the porous silicon for preparing in the prior art in the present invention, and luminous intensity not enough there is provided
A kind of hydrothermal preparing process of porous silica material.
In order to solve the above-mentioned technical problem, the present invention is addressed by following technical proposals：The hydro-thermal of porous silica material
Preparation method, comprises the following steps：
Cleaned after monocrystalline silicon piece ethanol, acetone soak；
Monocrystalline silicon piece is placed in the liner of hydrothermal reaction kettle after cleaning, etchant solution is injected within the liner；
Liner is put in hydrothermal reaction kettle shell, hydrothermal reaction kettle is placed in baking oven and carries out heating response, treats that its is anti-
It should terminate to be cooled to after room temperature, take out monocrystalline silicon piece and rinse well；
The monocrystalline silicon piece rinsed well takes out drying after hydrogen peroxide dipping；
The etchant solution injected in liner is mass fraction 30%-50% HF solution and concentration 0.3-1mol/L nitric acid
The volume ratio of zinc solution, HF solution and zinc nitrate solution is 2.5:1-6:1；The raw material of etchant solution is selected, matched and reaction bar
The part difference that to be the technical program maximum with prior art, using the composition of raw materials of art solutions etchant solution of the present invention
It is intended that expectation generates zinc oxide in porous silicon surface, increases the induction sensitivity to explosive, but obtain in many experiments
Porous silicon finished product detection have been surprisingly found that, using technical solution of the present invention, because of corruption of the zinc ion to monocrystalline silicon piece in etchant solution
Catalytic action is lost to obtain, the porous silicon of generation is provided with the advantages of high porosity, luminous intensity are high, surface apertures are homogeneous.
Preferably, baking oven heating-up temperature is 130 DEG C -160 DEG C, the time is 1-2 hours.
Preferably, the mass fraction 3% of hydrogen peroxide, soak time 1-3 days.
Preferably, monocrystalline silicon piece is the p type single crystal silicon piece of single-sided polishing, resistivity is 0.001-2 Ω/cm3.
The present invention is as a result of above technical scheme, and the porous silica material of preparation has significant technique effect：It is made
Porous silicon have the advantages that high porosity, luminous intensity be high, surface apertures are homogeneous；Rapid thermal oxidation need not be carried out, directly
With regard to obvious photic feux rouges phenomenon can be seen under uviol lamp.
The invention further relates to the preparation method of gas fluorescent optical sensor, for the porous of prior art gas fluorescent optical sensor
The phenomenon of blue shift occurs in silicon, and there is provided the preparation method of gas fluorescent optical sensor for the inadequate defect of luminous intensity.
In order to solve the above-mentioned technical problem, the present invention is addressed by following technical proposals：By fluorescence polymer solution
It is spun on the porous silica material that claim 1 or 2 or 3 or 4 is prepared, and 70 DEG C -100 DEG C dry 1-5 hours, fluorescence is high
Molecular solution is that fluorescence polymer material mixes to the solution obtained by dissolving, the matter of fluorescence polymer solution with chloroformic solution
It is 0.5-5mg/ml's to measure volume ratio.
Preferably, fluorescence polymer material using poly- [2- methoxyl groups -5- (2- ethyl hexyl oxies)-Isosorbide-5-Nitrae-phenylacetylene],
Poly- [2- methoxyl groups -5- (3 ', 7 '-dimethyl-octa epoxide) -1,4- phenylacetylenes], it is poly- [2,5- double (3 ', 7 '-dimethyl-octa epoxide) -
1,4- phenylenevinylenes], it is any in poly- [2- methoxyl groups -5- (2- ethyl hexyl oxies) -1,4- styrene].
The present invention is as a result of above technical scheme, and having obtained can be for the gas fluorescence sense that detects explosive
Device.The gas fluorescent optical sensor has following advantage：1st, the photoluminescence spectra of the hydro-thermal porous silicon is just high with fluorescence
The absorption spectrum of molecule is overlapping, occurs FRET phenomenons, as a result causes porous silicon light intensity to die down, the light intensity of fluorescence polymer increases
By force.2nd, the nano-pore aperture of hydro-thermal porous silicon surface is homogeneous, and the fluorescence for greatly adding the spin-coating film as substrate is passed
The homogeneity of sensor.3rd, the high-specific surface area of hydro-thermal porous silicon surface, high adsorption are that Fluorescent gas sensor is added and treated
The area of gas contact is surveyed, nano-porous surface also provides siphonage simultaneously so that the rate of adsorption is speeded.
In a word, the porous silicon prepared using technical solution of the present invention has fluorescence intensity as the gas fluorescent optical sensor of substrate
Height, film forming is homogeneous, and reference area is high, excellent adsorption, and with making that simple, cost is low, sensitivity is high, that reaction rate is fast is excellent
Point.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of porous silicon made from the embodiment of the present invention 1.
Fig. 2 is luminescence generated by light phenomenon comparison diagram of the porous silicon made from the embodiment of the present invention 1 under uviol lamp.
Fig. 3 is porous silicon pl figures made from the embodiment of the present invention 1 and gas Fluorescent gas sensor pl figures.
Fig. 4 is the pl figures of the TNT reactions of gas fluorescent optical sensor made from the embodiment of the present invention 1.
Embodiment
The present invention is described in further detail with reference to embodiment.
Embodiment 1
A kind of hydrothermal preparing process of porous silica material, preparation process is as follows：
Cleaned after monocrystalline silicon piece ethanol, acetone soak；In the present embodiment, monocrystalline silicon piece is 0.001-2 Ω/cm3 list
The p-type of mirror polish<100>Monocrystalline silicon piece, cleaning way is ultrasonic cleaning 10 minutes, then is rinsed 3-5 times repeatedly with distilled water.
Monocrystalline silicon piece is placed in the liner of hydrothermal reaction kettle after cleaning, etchant solution is injected within the liner；The present embodiment
In, mass fraction is 40% HF solution 30-50ml, and concentration is 0.3-1mol/L zinc nitrate 5-20ml etchant solutions.
Liner is put in hydrothermal reaction kettle shell, covers, tighten, hydrothermal reaction kettle is placed in baking oven and heat instead
Should, temperature is 140 DEG C, and the time is 1-2 hour, after its reaction end is cooled to room temperature, takes out monocrystalline silicon piece and rinses well；
Backwashing manner is to be rinsed repeatedly with distilled water.
The monocrystalline silicon piece rinsed well takes out drying after hydrogen peroxide dipping；The mass fraction of hydrogen peroxide is 3%, during immersion
Between be 1 day.
The preparation method of gas fluorescent optical sensor：Take poly- [2- methoxyl groups -5- (the 2- ethyl hexyls of appropriate high molecular fluorescent material
Epoxide)-Isosorbide-5-Nitrae-phenylacetylene], dissolved with chloroform solvent, mass volume ratio is 0.5-5mg/ml；Treat the poly- [2- of high molecular fluorescent material
Methoxyl group -5- (2- ethyl hexyl oxies) -1,4- phenylacetylenes] dissolve and completely afterwards revolved high molecular fluorescent material solvent using sol evenning machine
It is coated on porous silica material prepared by above-mentioned hydrothermal preparing process, is subsequently placed in 70-100 degree in baking oven, 1-5 hour.Produce
Gas fluorescent optical sensor by substrate of hydro-thermal porous silicon.
As Figure 1-4, it is the experimental result test chart of the present embodiment hydro-thermal porous silica material and gas fluorescent optical sensor,
As shown in figure 1, porous silicon surface has high porosity, the homogeneous advantage in nano-pore aperture；As shown in Fig. 2 through this patent skill
Porous silicon prepared by art scheme need not carry out rapid thermal oxidation, with regard to that can see that obvious photic feux rouges shows directly under uviol lamp
As；Experimental result as in Figure 2-4 shows, the absorption of the photoluminescence spectra of the hydro-thermal porous silicon just with fluorescence polymer
Spectra overlapping, occurs FRET phenomenons, as a result causes porous silicon light intensity to die down, the light intensity of fluorescence polymer is greatly enhanced, and hydro-thermal is more
High-specific surface area, the high adsorption of hole silicon face are that Fluorescent gas sensor adds the area contacted with test gas, nanometer
Porous surface also provides siphonage simultaneously so that the rate of adsorption is speeded.
Embodiment 2
Substantially the same manner as Example 1, it is quality point that it, which distinguishes the etchant solution for being to be injected in the liner of hydrothermal reaction kettle,
Number is 30% HF solution 50ml, and concentration is 0.3mol/L zinc nitrate 20ml；The temperature of baking oven heating hydrothermal reaction kettle is 160
DEG C, the time is 1 hour；Take out monocrystalline silicon piece to rinse well, flushing, which is put into after terminating in the hydrogen peroxide of mass fraction 3%, soaks
Drying is taken out after 2 days；High molecular fluorescent material is poly- [2- methoxyl groups -5- (3 ', 7 '-dimethyl-octa epoxide) -1,4- phenylacetylenes].
The technique effect of the present embodiment is substantially the same manner as Example 1.
Embodiment 3
Substantially the same manner as Example 1, it is quality point that it, which distinguishes the etchant solution for being to be injected in the liner of hydrothermal reaction kettle,
Number is 30% HF solution 60ml, and concentration is 1mol/L zinc nitrate 10ml；The temperature of baking oven heating hydrothermal reaction kettle is 130
DEG C, the time is 2 hours；Reaction end is cooled to after room temperature, is taken out monocrystalline silicon piece and is rinsed well, flushing is put into quality after terminating
Drying is taken out after being soaked 3 days in the hydrogen peroxide of fraction 3%；High molecular fluorescent material is poly- [double (3 ', the 7 '-dimethyl-octa oxygen of 2,5-
Base) -1,4- phenylenevinylenes].
The technique effect of the present embodiment is substantially the same manner as Example 1.
In a word, presently preferred embodiments of the present invention, all equalizations made according to scope of the present invention patent be the foregoing is only
Change and modification, should all belong to the covering scope of patent of the present invention.
Claims (6)
1. the hydrothermal preparing process of porous silica material, comprises the following steps：
Cleaned after monocrystalline silicon piece ethanol, acetone soak；
Monocrystalline silicon piece is placed in the liner of hydrothermal reaction kettle after cleaning, etchant solution is injected within the liner；
Liner is put in hydrothermal reaction kettle shell, hydrothermal reaction kettle is placed in baking oven and carries out heating response, its reaction knot is treated
Beam is cooled to after room temperature, is taken out monocrystalline silicon piece and is rinsed well；
The monocrystalline silicon piece rinsed well takes out drying after hydrogen peroxide dipping；
It is characterized in that：Etchant solution is that mass fraction 30%-50% HF solution and concentration 0.3-1mol/L zinc nitrate are molten
The volume ratio of liquid, HF solution and zinc nitrate solution is 2.5:1-6:1.
2. the hydrothermal preparing process of porous silica material according to claim 1, it is characterised in that：Baking oven heating-up temperature is
130 DEG C -160 DEG C, the time is 1-2 hours.
3. the hydrothermal preparing process of porous silica material according to claim 1, it is characterised in that：The mass fraction of hydrogen peroxide
For 3%, soak time 1-3 days.
4. the hydrothermal preparing process of porous silica material according to claim 1, it is characterised in that：Monocrystalline silicon piece is thrown for one side
The p type single crystal silicon piece of light, resistivity is 0.001-2 Ω/cm3.
5. the preparation method of gas fluorescent optical sensor, it is characterised in that：Fluorescence polymer solution is spun to claim 1 or 2
Or 3 or 4 on the porous silica material prepared, and 70 DEG C -100 DEG C dry 1-5 hours, fluorescence polymer solution is fluorescence high score
Sub- material mixes to the solution obtained by dissolving with chloroformic solution, and the mass volume ratio of fluorescence polymer solution is 0.5-5mg/
ml。
6. the preparation method of gas fluorescent optical sensor according to claim 5, it is characterised in that：Fluorescence polymer material is adopted
With poly- [2- methoxyl groups -5- (2- ethyl hexyl oxies) -1,4- phenylacetylenes], poly- [2- methoxyl groups -5- (3 ', 7 '-dimethyl-octa oxygen
Base) -1,4- phenylacetylenes], poly- [2,5- double (3 ', 7 '-dimethyl-octa epoxide) -1,4- phenylenevinylenes], it is poly- [2- methoxyl groups -
5- (2- ethyl hexyl oxies) -1,4- styrene] in it is any.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111172597A (en) * | 2020-01-21 | 2020-05-19 | 河南理工大学 | Preparation method of luminescent porous silicon |
| CN113638053A (en) * | 2021-08-09 | 2021-11-12 | 杭州芬得检测技术有限公司 | Preparation method of porous black silicon material, preparation method of fluorescent sensor and method for detecting explosive by using fluorescent sensor |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1241611A (en) * | 1998-07-09 | 2000-01-19 | 中国科学技术大学 | Hydrothermal preparation process of luminous iron-deactivated porous silicon |
| US20080069756A1 (en) * | 2005-01-27 | 2008-03-20 | Fumitaka Kume | Preferential Etching Method and Silicon Single Crystal Substrate |
| US20100301276A1 (en) * | 2009-05-27 | 2010-12-02 | Joong Kee Lee | Method of preparing bundle type silicon nanorod composite through electroless etching process using metal ions and anode active material for lithium secondary cells comprising the same |
| CN102391014A (en) * | 2011-08-12 | 2012-03-28 | 华北水利水电学院 | Active substrate with surface enhanced Raman scattering effect |
| CN103865180A (en) * | 2012-12-12 | 2014-06-18 | 中国石油化工股份有限公司 | Luminescent composite material and preparation method thereof |
| CN105970278A (en) * | 2016-04-27 | 2016-09-28 | 杭州芬得检测技术有限公司 | Preparation method of porous silicon material |
-
2017
- 2017-04-28 CN CN201710293877.8A patent/CN107188184B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1241611A (en) * | 1998-07-09 | 2000-01-19 | 中国科学技术大学 | Hydrothermal preparation process of luminous iron-deactivated porous silicon |
| US20080069756A1 (en) * | 2005-01-27 | 2008-03-20 | Fumitaka Kume | Preferential Etching Method and Silicon Single Crystal Substrate |
| US20100301276A1 (en) * | 2009-05-27 | 2010-12-02 | Joong Kee Lee | Method of preparing bundle type silicon nanorod composite through electroless etching process using metal ions and anode active material for lithium secondary cells comprising the same |
| CN102391014A (en) * | 2011-08-12 | 2012-03-28 | 华北水利水电学院 | Active substrate with surface enhanced Raman scattering effect |
| CN103865180A (en) * | 2012-12-12 | 2014-06-18 | 中国石油化工股份有限公司 | Luminescent composite material and preparation method thereof |
| CN105970278A (en) * | 2016-04-27 | 2016-09-28 | 杭州芬得检测技术有限公司 | Preparation method of porous silicon material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111172597A (en) * | 2020-01-21 | 2020-05-19 | 河南理工大学 | Preparation method of luminescent porous silicon |
| CN111172597B (en) * | 2020-01-21 | 2021-03-26 | 河南理工大学 | Preparation method of luminescent porous silicon |
| CN113638053A (en) * | 2021-08-09 | 2021-11-12 | 杭州芬得检测技术有限公司 | Preparation method of porous black silicon material, preparation method of fluorescent sensor and method for detecting explosive by using fluorescent sensor |
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Effective date of registration: 20221228 Address after: 101500 room 5206, building 17, 18 Yuanyuan Road, economic development zone, Miyun District, Beijing Patentee after: FOUNDMACRO Co.,Ltd. Address before: 311100 Room 492, Building 3, No. 1, Lvting Road, Cangqian Street, Yuhang District, Hangzhou City, Zhejiang Province Patentee before: FINDER DETECTION TECHNOLOGIES CO.,LTD. |
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Effective date of registration: 20230411 Address after: 310000 east side of the second floor of Building 2, No. 11-1, Yuda Road, Yuhang street, Yuhang District, Hangzhou City, Zhejiang Province Patentee after: FINDER DETECTION TECHNOLOGIES CO.,LTD. Address before: 101500 room 5206, building 17, 18 Yuanyuan Road, economic development zone, Miyun District, Beijing Patentee before: FOUNDMACRO Co.,Ltd. |