CN103088297A - Method and device for preparing silver black nanoparticles on porous surface of nuclear track - Google Patents
Method and device for preparing silver black nanoparticles on porous surface of nuclear track Download PDFInfo
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- CN103088297A CN103088297A CN2011103326447A CN201110332644A CN103088297A CN 103088297 A CN103088297 A CN 103088297A CN 2011103326447 A CN2011103326447 A CN 2011103326447A CN 201110332644 A CN201110332644 A CN 201110332644A CN 103088297 A CN103088297 A CN 103088297A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 83
- 239000004332 silver Substances 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 36
- 229920000728 polyester Polymers 0.000 claims abstract description 47
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 238000002360 preparation method Methods 0.000 claims abstract description 24
- 229910052786 argon Inorganic materials 0.000 claims abstract description 22
- 229910052751 metal Inorganic materials 0.000 claims abstract description 14
- 239000002184 metal Substances 0.000 claims abstract description 14
- 238000005530 etching Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims description 24
- 230000008020 evaporation Effects 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 14
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 14
- 229910052721 tungsten Inorganic materials 0.000 claims description 14
- 239000010937 tungsten Substances 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 239000010931 gold Substances 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 229920006267 polyester film Polymers 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 239000011358 absorbing material Substances 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 238000007747 plating Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000009189 diving Effects 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910001935 vanadium oxide Inorganic materials 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- DIOZVWSHACHNRT-UHFFFAOYSA-N 2-(2-prop-2-enoxyethoxy)ethanol Chemical compound OCCOCCOCC=C DIOZVWSHACHNRT-UHFFFAOYSA-N 0.000 description 1
- -1 Glycol Carbonates Chemical class 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- POQKXAGEBNZGTF-UHFFFAOYSA-N [C].CC(O)=O Chemical compound [C].CC(O)=O POQKXAGEBNZGTF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
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- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to a preparation technology of a silver black nano material, in particular to a method and a device for preparing silver black nano particles on a nuclear track porous surface. The method comprises32S ions irradiate the polyester or CR-39 sample, and a nuclear track polyester sample or a nuclear track CR-39 sample is obtained through a NaOH solution etching process; adhering the nuclear track polyester sample or the nuclear track CR-39 sample and the detector sheet on a sample rack in a vacuum chamber to make the pressure in the vacuum chamber reach 3 x 10-3-4×10-3Pa; filling argon into the vacuum cavity to ensure that the pressure of the argon in the vacuum cavity is 50-100 Pa; heating the silver wire in the vacuum chamber to melt and evaporate the silver, and plating a layer of metal silver on the surface of the nuclear track polyester sample or the nuclear track CR-39 sampleAnd (3) nanoparticles. The invention provides a new thought and method for preparing the infrared thermosensitive sensor absorbing material silver black, and has a revelation effect on more efficient utilization of an infrared detector.
Description
Technical field
The present invention relates to the black preparations of nanomaterials technology of silver, be specifically related to method and device that a kind of nuclear track porous surface prepares the black nano particle of silver.
Background technology
Infrared eye such as thermoelectricity type infrared eye, air-driven type infrared eye, thermosensitive resistance type infrared eye and thermoviewer etc. have obtained studying widely and using in military and national defense and civil area, especially under the promotion of the traction of military requirement and correlation technique development, infrared detection technique as new and high technology will be more extensive in the application in future, and the status is more important.The core component of infrared eye is the infra-red heat dependent sensor.Only have the heat sensitive sensor of working as effectively and in time to transmit the heat of sensing, infrared eye just has response.Therefore require the absorption layer of temperature-sensitive tactility apparatus to photo-thermal, very high sensitivity must be arranged.Conventional absorption layer material such as vanadium oxide, metallic substance (Ni, Cr and Au etc.) and amorphous semiconductor etc. have better performance, are best but do not have a kind of.The electrical resistance temperature of metal and changing, vanadium oxide is not suitable for integrated circuit technique, and amorphous semiconductor is attended by a large amount of low frequency noises.The black nano particle of metal current is considered to make up above shortcoming, is fit to very much do the absorption layer of heat sensitive sensor and the focus that becomes research.So-called metal black (metal black) is certain metallic substance with nanoscale porous colloidal (as black in gold, silver is black, platinum black, carbon black etc.), is the gathering pattern of metal nano group.The nano metal cluster is the surface that the porous pattern makes material and becomes coarse.Therefore the micro interface of uneven surface has the interface normal of different orientation, and large surface-area and complicated tortuous reflected light path are arranged, and can make incident electromagnetic wave generation scattering and decay, reduces its specular reflection and promotes photo-thermal and transform.
The method for making of metal nano grade particles generally has rare gas element method of evaporation, rare gas element using vaporization condensation process and some electro-plating methods.The above two are all to make at the lower evaporated metal of rough vacuum atmosphere (nitrogen, argon gas), the rare gas element using vaporization condensation process than more than the rare gas element method of evaporation to the setting of the substrate active cooling that will deposit.At present, many about research and the report of the black nano particle of gold.J.Lehman etc. are under 130Pa and 260Pa nitrogen pressure, at LiTaO
3Having prepared diameter on substrate, to be about the gold of 10 microns black.Roberto R Neli etc. are at 2*10
-4-10*10
-4Under the nitrogen pressure of Pa, prepared diameter black between the gold of 0.1-1 micron on silicon substrate.Just simply mention in the document that can find at present and prepare silver-colored black method, the instrument and the process that also do not have the detailed report of document or description preparation silver to deceive.
Summary of the invention
The object of the present invention is to provide preparation method and the device of the black nano particle of a kind of silver, syncaryon track vesicular structure and Yin Hei nanoporous characteristic are under certain ar pressure, at the black nano particle of nuclear track porous surface preparation silver.
Technical scheme of the present invention is as follows: a kind of nuclear track porous surface prepares the method for the black nano particle of silver, comprises the steps:
(S1) pass through
32The polyester that S ion irradiation 20-50 μ m is thick or the thick CR-39 sample of 0.5-2mm obtain nuclear track polyester sample or nuclear track CR-39 sample through NaOH solution etch process;
(S2) with the nuclear track polyester sample or the nuclear track CR-39 sample that obtain in step (S1), and stick to the interior specimen holder of vacuum chamber for the detector sheet of demarcating the black thickness of silver, make the interior pressure of vacuum chamber reach 3 * 10
-3-4 * 10
-3Pa;
(S3) be filled with argon gas in vacuum chamber, making the ar pressure in vacuum chamber is 50-100Pa;
(S4) filamentary silver in the heating, vacuum chamber, make silver dissolve evaporation, plates the layer of metal silver nano-grain in nuclear track polyester sample or nuclear track CR-39 sample surfaces.
Further, nuclear track porous surface as above prepares the method for the black nano particle of silver, and the concrete grammar that obtains nuclear track polyester sample or nuclear track CR-39 sample in step (S1) is as follows:
(a) pass through
32The polyester that S ion irradiation 20-50 μ m is thick or the thick CR-39 sample of 0.5-2mm, irradiation density is 10
8-10
9Individual/cm
2, irradiation time is 30-60 minute;
(b) irradiated sample is placed in the dry environment 1-3 of cleaning month;
(c) be NaOH solution etching 2-8 minute of 6.0-6.5Mol/L with the sample concentration after standing 1-3 month, etch temperature is 55-70 ℃;
(d) with sample 2-6 hour after etching in 300-360nm ultra violet lamp step (c);
(e) the NaOH solution etching that is 6.0-6.5Mol/L with postradiation sample concentration in step (d) 10-25 minute, etch temperature is 55-70 ℃;
(f) etch processes sample is later fully dried.
Further, nuclear track porous surface as above prepares the method for the black nano particle of silver, and wherein, described polyester can be biaxially oriented polyester film Mylar20, Mylar50, perhaps the Melinex polyester of other kinds, Hostaphan polyester.
Further, nuclear track porous surface as above prepares the method for the black nano particle of silver, and selecting thickness for the detector sheet of demarcating the black thickness of silver in step (S2) is aluminium flake or gold plaque or the copper sheet of 0.5-1mm.
Further, nuclear track porous surface as above prepares the method for the black nano particle of silver, and in step (S4), the filamentary silver of heating evaporation and the distance between nuclear track polyester sample or nuclear track CR-39 sample are 7-10cm.
The device of the black nano particle of a kind of nuclear track porous surface preparation silver, comprise the evaporation coating machine, the evaporation coating machine is provided with vacuum chamber, vacuum chamber is connected with argon supply system, wherein, be provided with specimen holder in described vacuum chamber, specimen holder is provided with nuclear track polyester sample or nuclear track CR-39 sample, and the detector sheet that is used for demarcating the black thickness of silver; Be provided with the tungsten boat that is connected with the electrode of evaporation coating machine below specimen holder, be placed with filamentary silver on the tungsten boat.
Further, the device of the black nano particle of nuclear track porous surface preparation silver as above, wherein, described nuclear track polyester sample or nuclear track CR-39 sample and detector sheet are located at respectively take tungsten boat medullary ray on the symmetric position of axle.
Further, the device of the black nano particle of nuclear track porous surface preparation silver as above wherein, is being provided with shielding case above described filamentary silver and between specimen holder.
Further, the device of the black nano particle of nuclear track porous surface preparation silver as above, wherein, described detector sheet is the circular aluminium flake of diameter 20mm, its thickness is 1mm.
Beneficial effect of the present invention is as follows: the present invention combines nuclear track vesicular structure and Yin Hei nanoporous characteristic, under the 50-100Pa ar pressure, has prepared silver-colored black nano particle at the nuclear track porous surface.The present invention utilizes infrared eye to have the enlightenment effect for the black preparation of infra-red heat dependent sensor absorbing material silver provides a kind of new thinking and method more efficiently.
Description of drawings
Fig. 1 is the apparatus structure schematic diagram of the black nano particle of nuclear track porous surface preparation silver of the present invention;
Fig. 2 is the method flow diagram of the black nano particle of nuclear track porous surface preparation silver of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in detail.
This acid propylene of CR-39 formal name used at school carbon acetic acid, or claim allyl diglycol acid fat (Dially Glycol Carbonates), be to use resin material very widely.The present invention utilizes
32S ion irradiation CR-39 sample or polyester sample produce the track of diving; Adopt pre-etching sensitization etched experimental technique etch processes CR-39 sample or polyester sample again, make the track of diving become the hole of micrometer/nanometer; Utilize the rare gas element method of evaporation, under certain ar pressure, plate the metal silver nano-grain at sample surfaces.When adopting polyester sample, can select biaxially oriented polyester film (BoPET) Mylar20, Mylar50, the perhaps polyester of other kinds, as Melinex, Hostaphan etc.
The device of the black nano particle of nuclear track porous surface preparation silver provided by the present invention as shown in Figure 1, its basic structure comprises evaporation coating machine 1, evaporation coating machine 1 is provided with vacuum chamber 2, vacuum chamber 2 is connected with argon supply system 3, argon supply system 3 is regulated the flow of argon gas by argon flow amount controller 13, argon flow amount controller 13 can be controlled by coarse adjustment and fine setting the flow of argon gas.Also connect the pressure detecting instrument 12 for detection of pressure on vacuum chamber 2.Be provided with specimen holder 4 in described vacuum chamber 2, specimen holder 4 is provided with nuclear track polyester sample or nuclear track CR-39 sample 6, and (two kinds of samples can be selected one, the position that arranges is identical), and the detector sheet 5 that is used for demarcating the black thickness of silver, it is aluminium flake or gold plaque or the copper sheet of 0.5-1mm that the detector sheet can be selected thickness.Be provided with the tungsten boat 10 that is connected with the electrode of evaporation coating machine 1 below specimen holder 4, tungsten boat 10 is located between the negative electrode 8 and anode 9 of evaporation coating machine 1, be placed with high-purity filamentary silver 7 on the tungsten boat, the distance between filamentary silver 7 and nuclear track polyester sample or nuclear track CR-39 sample 6 is 7-10cm.The ship type container that tungsten boat 10 is made with high pure metal tungsten sheet exactly is used as the thermal resistance evaporation boat, makes filamentary silver melt evaporation by heating tungsten boat.Be provided with shielding case 11 above filamentary silver 7 and between specimen holder 4, shielding case 11 is for shielding sample when heating filamentary silver, in order to avoid the fusing of the high temperature that the nuclear track film sample is splashed silver or damage.Shielding case 11 is connected with vacuum chamber 2 transmission shaft (not shown in FIG.) outward, and the handle on rotating drive shaft top just can mobile shielding case outside.After finding that from viewing window filamentary silver is melted fully, then remove shielding case 11 by the handle of operation transmission shaft, the black process of Evaporation preparation silver just formally begins.In the present embodiment, the detector sheet in vacuum chamber 2 is that thickness is the aluminium flake 5 of 1mm, and aluminium flake is the circular piece of diameter 20mm, is used for demarcating the black thickness of silver.Nuclear track polyester sample or nuclear track CR-39 sample 6 are located at respectively take tungsten boat medullary ray on the symmetric position of axle with detector sheet 5.Detector sheet 5 is accurately measured weight before and after the black nano particle of preparation silver, with the black thickness of silver on weight difference and density formula calculating detector sheet surface.Because the environment in vacuum chamber is isotropic, therefore, it is identical in theory that the black thickness of the silver on the detector sheet is deceived thickness with the silver on sample.
Use method flow that said apparatus realizes the black nano particle of nuclear track porous surface preparation silver as shown in Figure 2, comprise the steps:
Step S1, by
32The polyester that S ion irradiation 20-50 μ m is thick or the thick CR-39 sample of 0.5-2mm obtain nuclear track polyester sample or nuclear track CR-39 sample through NaOH solution etch process.
The present embodiment is that the energy that utilizes China Atomic Energy Science Research Institute's HI-13 tandem accelerator to provide is strong for 10nA-20nA's for 80-100MeV, stream
32The polyester that S ion irradiation 20-50 μ m is thick or the thick CR-39 sample of 0.5-2mm, irradiation density is 10
8-10
9Individual/cm
2, irradiation time is 30-60 minute.Certainly, those skilled in the art also can adopt other radioactive source to carry out irradiation.In the present embodiment, that polyester is selected is biaxially oriented polyester film (BoPET) Mylar20, Mylar50, certainly, also can select the polyester of other kinds, as Melinex, and Hostaphan etc.Polyester and CR-39 resin material all can be used as nuclear track hole substrate material, and optional one gets final product in preparation process.The concrete thickness of polyester and CR-39 can be determined in corresponding thickness range as required.
After irradiated sample is placed in the dry environment 1-3 of cleaning month, be NaOH solution etched sample 2-8 minute of 6.0-6.5Mol/L with concentration, etched temperature is 55-70 ℃.Next, with sample 2-6 hour after the etching of 300-360nm ultra violet lamp.At last, then the NaOH solution etching 10-25 that is 6.0-6.5Mol/L with concentration divides, and etched temperature is 55-70 ℃.After etch processes, sample is placed on and is used further to prepare silver-colored deceiving after loft drier (temperature 30-40 ℃) fully dried in middle 48-60 hour.
Step S2 with nuclear track polyester sample or the nuclear track CR-39 sample that obtains in step S1, and sticks to the interior specimen holder of vacuum chamber for the detector sheet of demarcating the black thickness of silver, makes the interior pressure of vacuum chamber reach 3 * 10
-3-4 * 10
-3Pa.
After sticking to nuclear track polyester sample or nuclear track CR-39 sample and detector sheet on specimen holder in vacuum chamber, the vacuum system that namely can open the evaporation coating machine, the pressure in vacuum chamber reaches 3*10
-3-4*10
-3During Pa, close the Link Port of vacuum chamber and coating equipment host computer system.The best plan of establishment of sample and detector sheet is to be located at respectively take tungsten boat medullary ray on the symmetric position of axle, can make like this sample more consistent with the black thickness of silver on the detector sheet.It is aluminium flake or gold plaque or the copper sheet of 0.5-1mm that the detector sheet can be selected thickness, and the detector sheet of the present embodiment is that thickness is the circular aluminium flake of 1mm, diameter 20mm.
Step S3 is filled with argon gas in vacuum chamber, making the ar pressure in vacuum chamber is 50-100Pa.
Open argon supply system, regulate the flow of argon gas by the argon flow amount controller, making the pressure of argon gas in vacuum chamber is 50-100Pa, closes argon supply system.Pressure in vacuum chamber carries out real-time detection by external pressure detecting instrument.
Step S4, the filamentary silver in the heating, vacuum chamber makes silver dissolve evaporation, plates the layer of metal silver nano-grain in nuclear track polyester sample or nuclear track CR-39 sample surfaces.
Open electrode supply, the black nano particle of preparation silver.Filamentary silver dissolves under the heat effect of electrode, at this moment, block above filamentary silver with shielding case, in order to avoid the fusing of the high temperature that the nuclear track film sample is splashed silver or damage, after finding that from the viewing window of vacuum chamber filamentary silver is melted fully, handle by the transmission shaft top that is connected with shielding case in vacuum chamber outside rotation, shielding case is removed directly over filamentary silver, thereby, the silver-colored steam that dissolves evaporation upwards diffuses on the nuclear track polyester sample or nuclear track CR-39 sample of specimen holder, and on the detector sheet, the black process of Evaporation preparation silver just formally begins.Keep a close eye on the indication of external pressure detecting instrument in preparation process, if lower than predetermined argon pressure, open immediately argon supply system and be filled with argon gas, make pressure reach preset value.
Deceive at the silver of nuclear track CR-39 sample or the surface preparation of nuclear track polyester sample by aforesaid method and be spherical cluster, diameter can reach 3 μ m.Spherical cluster is that single nanoparticle forms, and the diameter of single nanoparticle is about 60～100nm.Measure the reflectivity of plated film sample in infrared light district (2.5～25 μ m), measuring result shows, the nuclear track of CR-39 sample surfaces and silver nano-grain can be reduced to 0.9% with the reflectivity in infrared light district (8.0～25 μ m), with the CR-39 comparison of non-modified, have lowered 82%.At 5.8 and 7.8 μ m places, the background reflection of CR-39 has been reduced to 5.0% and 6.8% from 9.0% and 13.0% respectively.
Obviously, those skilled in the art can carry out various changes and modification and not break away from the spirit and scope of the present invention the present invention.Like this, if of the present invention these are revised and within modification belongs to the scope of claim of the present invention and equivalent technology thereof, the present invention also is intended to comprise these changes and modification interior.
Claims (9)
1. a nuclear track porous surface prepares the method that silver is deceived nano particle, comprises the steps:
(S1) pass through
32The polyester that S ion irradiation 20-50 μ m is thick or the thick CR-39 sample of 0.5-2mm obtain nuclear track polyester sample or nuclear track CR-39 sample through NaOH solution etch process;
(S2) with the nuclear track polyester sample or the nuclear track CR-39 sample that obtain in step (S1), and stick to the interior specimen holder of vacuum chamber for the detector sheet of demarcating the black thickness of silver, make the interior pressure of vacuum chamber reach 3 * 10
-3-4 * 10
-3Pa;
(S3) be filled with argon gas in vacuum chamber, making the ar pressure in vacuum chamber is 50-100Pa;
(S4) filamentary silver in the heating, vacuum chamber, make silver dissolve evaporation, plates the layer of metal silver nano-grain in nuclear track polyester sample or nuclear track CR-39 sample surfaces.
2. nuclear track porous surface as claimed in claim 1 prepares the method for the black nano particle of silver, and it is characterized in that: the concrete grammar that obtains nuclear track polyester sample or nuclear track CR-39 sample in step (S1) is as follows:
(a) pass through
32The polyester that S ion irradiation 20-50 μ m is thick or the thick CR-39 sample of 0.5-2mm, irradiation density is 10
8-10
9Individual/cm
2, irradiation time is 30-60 minute;
(b) irradiated sample is placed in the dry environment 1-3 of cleaning month;
(c) be NaOH solution etching 2-8 minute of 6.0-6.5Mol/L with the sample concentration after standing 1-3 month, etch temperature is 55-70 ℃;
(d) with sample 2-6 hour after etching in 300-360nm ultra violet lamp step (c);
(e) the NaOH solution etching that is 6.0-6.5Mol/L with postradiation sample concentration in step (d) 10-25 minute, etch temperature is 55-70 ℃;
(f) etch processes sample is later fully dried.
3. nuclear track porous surface as claimed in claim 2 prepares the method for the black nano particle of silver, and it is characterized in that: described polyester can be biaxially oriented polyester film Mylar20, Mylar50, perhaps Melinex polyester, Hostaphan polyester.
4. nuclear track porous surface as claimed in claim 1 prepares the method for the black nano particle of silver, it is characterized in that: selecting thickness for the detector sheet of demarcating the black thickness of silver in step (S2) is aluminium flake or gold plaque or the copper sheet of 0.5-1mm.
5. nuclear track porous surface as described in any one in claim 1-4 prepares the method for the black nano particle of silver, it is characterized in that: in step (S4), the filamentary silver of heating evaporation and the distance between nuclear track polyester sample or nuclear track CR-39 sample are 7-10cm.
6. a nuclear track porous surface prepares the device that silver is deceived nano particle, comprise evaporation coating machine (1), evaporation coating machine (1) is provided with vacuum chamber (2), vacuum chamber (2) is connected with argon supply system (3), it is characterized in that: be provided with specimen holder (4) in described vacuum chamber (2), specimen holder (4) is provided with nuclear track polyester sample or nuclear track CR-39 sample (6), and the detector sheet (5) that is used for demarcating the black thickness of silver; Be provided with the tungsten boat (10) that is connected with the electrode (8,9) of evaporation coating machine (1) in the below of specimen holder (4), be placed with filamentary silver (7) on tungsten boat (10).
7. the device of the black nano particle of nuclear track porous surface as claimed in claim 6 preparation silver is characterized in that: described nuclear track polyester sample or nuclear track CR-39 sample (6) and detector sheet (5) are located at respectively medullary ray take tungsten boat (10) on the symmetric position of axle.
8. the device of the black nano particle of nuclear track porous surface preparation silver as claimed in claim 6, is characterized in that: be provided with shielding case (11) between described filamentary silver (7) top and specimen holder (4).
9. as the device of claim 6 or the 7 or 8 black nano particles of described nuclear track porous surface preparation silver, it is characterized in that: described detector sheet (5) is the circular aluminium flake of diameter 20mm, and its thickness is 1mm.
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| CN2011103326447A CN103088297A (en) | 2011-10-28 | 2011-10-28 | Method and device for preparing silver black nanoparticles on porous surface of nuclear track |
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|---|---|---|---|
| CN2011103326447A CN103088297A (en) | 2011-10-28 | 2011-10-28 | Method and device for preparing silver black nanoparticles on porous surface of nuclear track |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107287598A (en) * | 2017-07-19 | 2017-10-24 | 枣庄惠风能源科技有限公司 | A kind of preparation method of heavy ion nucleopore copper foil |
| CN113270538A (en) * | 2020-12-29 | 2021-08-17 | 有研工程技术研究院有限公司 | Infrared detector sensitive element based on nano infrared absorption layer and preparation method thereof |
| CN113354018A (en) * | 2021-07-09 | 2021-09-07 | 中国科学院近代物理研究所 | Solar evaporation hierarchical structure and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107287598A (en) * | 2017-07-19 | 2017-10-24 | 枣庄惠风能源科技有限公司 | A kind of preparation method of heavy ion nucleopore copper foil |
| CN113270538A (en) * | 2020-12-29 | 2021-08-17 | 有研工程技术研究院有限公司 | Infrared detector sensitive element based on nano infrared absorption layer and preparation method thereof |
| CN113354018A (en) * | 2021-07-09 | 2021-09-07 | 中国科学院近代物理研究所 | Solar evaporation hierarchical structure and preparation method thereof |
| CN113354018B (en) * | 2021-07-09 | 2023-10-24 | 中国科学院近代物理研究所 | Solar evaporation hierarchical structure and preparation method thereof |
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