CN106835110B - A kind of environment-friendly type antiradar reflectivity membrane material and preparation method thereof - Google Patents
A kind of environment-friendly type antiradar reflectivity membrane material and preparation method thereof Download PDFInfo
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- CN106835110B CN106835110B CN201710058327.8A CN201710058327A CN106835110B CN 106835110 B CN106835110 B CN 106835110B CN 201710058327 A CN201710058327 A CN 201710058327A CN 106835110 B CN106835110 B CN 106835110B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
- C23C22/62—Treatment of iron or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
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Abstract
The environment-friendly type antiradar reflectivity membrane material and preparation method thereof of in-situ self-grown, belongs to environment-friendly type antiradar reflectivity membrane material preparation technical field in a kind of ferrochrome substrate.It is made of ferrochrome piece substrate and spinel particles low-reflection film layer, spinel particles Fe of the low-reflection film layer by size in 0.09~1.9 μm of section2.58~ 2.59Cr0.28~0.30O4It piles up.It is to wipe ferrochrome substrate surface with alcohol swab, keeps surface smooth clean；Substrate is put into the mixed solution of 80mL dehydrated alcohol, glycerol, KOH and deionized water；Substrate and mixed solution are fitted into the reaction kettle of polytetrafluoroethyllining lining together, 10~48h is reacted under the conditions of 180~240 DEG C；Be cooled to room temperature after reaction kettle is taken out, then by reaction system ultrasound, be filtered, washed after be dried at 30~100 DEG C, to obtain environment-friendly type antiradar reflectivity membrane material.The present invention has the characteristics that preparation is simple, raw material is cheap, treatment process is easy, and membrane material can be applied to the fields such as photothermal conversion and infrared spectrometer.
Description
Technical field
The invention belongs to environment-friendly type antiradar reflectivity membrane material preparation technical fields, and in particular in a kind of ferrochrome substrate
Environment-friendly type antiradar reflectivity membrane material of in-situ self-grown and preparation method thereof.
Background technique
Reflectivity has important application at many aspects less than 10% low reflectivity material.Especially environment-friendly type is low
Reflectivity membrane material, it facilitates photothermal conversion, and can be used for the fields such as spectrometer.
A variety of micro-nano crystal grain have been used for constructing environment-friendly type antiradar reflectivity membrane material, and the means of preparation have wet chemistry quarter
Erosion, chemical dry etching, laser ablation, spin-coating method etc..The more environmental protection of ferrochrome substrate is cheap, as environment-friendly type antiradar reflectivity
The raw material of membrane material, is easy to large scale preparation.It is easily prepared under suitable solution ratio with the raw material by hydro-thermal reaction
AB containing Fe, Cr element2O4Spinel, and obtain near ultraviolet visible and near infrared spectrum area (300~2500nm) lower
Reflectivity.The preparation method is at low cost, and raw material sources are wide, and pre-treatment convenient post-treatment, required equipment is simple, has larger popularization
Prospect.
Summary of the invention
The object of the present invention is to provide a kind of environment-friendly type antiradar reflectivity membrane materials and preparation method thereof.Ring of the present invention
Guarantor's type antiradar reflectivity membrane material is made of ferrochrome piece substrate and spinel particles low-reflection film layer, can be at 180~240 DEG C
Mixed solution in prepared, by adjusting heating temperature, heating time, mixed solution proportion can obtain different crystal grain and arrange
The environment-friendly type antiradar reflectivity membrane material of column-shaped state.By icp analysis result it is found that prepared low-reflection film layer by size 0.09
The spinel particles Fe in~1.9 μm of sections2.58~2.59Cr0.28~0.30O4It piles up.
Environment-friendly type antiradar reflectivity membrane material of the present invention has a characteristic that preparation is simple, and raw material is cheap, processes
Journey is easy, very promising, and can be applied to the reflection-reducing material of spectrometer box house.
The ferrochrome substrate be commercial goods, by mass percentage, contain Cr:11%, Fe:88%, 0 < Cu <
0.1%, 0 < Mn < 0.1%, 0 < Ni < 0.1%, 0 < P < 0.05%, 0 < Mo < 0.1%, 0 < Si < 0.1%, 0 < C < 0.4%, substrate are thick
Degree is 0.2~10mm (different substrate thickness influences the performance of membrane material little).The surface of substrate does not need to carry out additional
Polishing treatment.
A kind of preparation method of environment-friendly type antiradar reflectivity membrane material of the present invention, its step are as follows:
(1) ferrochrome substrate surface is wiped with alcohol swab, keeps surface smooth clean；
(2) substrate is put into 80mL mixed solution, the group of the mixed solution becomes 10~15mL dehydrated alcohol, 1~2mL
Glycerol and 22.4g-44.8gKOH, remaining is deionized water；
(3) substrate and mixed solution are fitted into together in the reaction kettle of polytetrafluoroethyllining lining, in 180~240 DEG C of conditions
10~48h of lower reaction；
(4) be cooled to room temperature after taking out reaction kettle, then by reaction system 1~12h of ultrasound, then to ultrasonic product into
Row filtering, then filtration product is washed with deionized, (drying temperature is dried at 30~100 DEG C in last washed product
The performance of membrane material is influenced little), to obtain environment-friendly type antiradar reflectivity membrane material of the present invention.
The environment-friendly type antiradar reflectivity membrane material can be by adjusting preparation temperature, the proportion of mixed reaction solution, preparation time
Etc. obtaining the spinel particles with different ordered states, and then obtain the antiradar reflectivity membrane material of the environment-friendly type of different performance
Material.
The environment-friendly type antiradar reflectivity membrane material passes through hydro-thermal method growth in situ in the substrate of ferrochrome, the material
Low principle of reflection can be explained as follows: the spinel films mainly pass through different scale spinel particles constitute it is multiple dimensioned
Multipath reflection and absorption to incident ray are realized in micropore, are finally reached the purpose of low reflection.The membrane material can also be with simultaneously
It is considered as effective optical medium of air filling, gradually changed refractive index feature is conducive to the absorption to incident light.In addition the material
The surface-interface effect and dielectric effect of nanocrystal also contribute to forming the low reflection of high-selenium corn.
Environment-friendly type antiradar reflectivity membrane material of the invention has following advantage:
The preparation cost of the environment-friendly type antiradar reflectivity membrane material is low, and raw material is cheap, and treatment process is simple, does not need complicated instrument
Device equipment has market prospects, has preferable application value in optothermal material and infrared spectrometer field.
Detailed description of the invention
Fig. 1: environment-friendly type antiradar reflectivity membrane material structural schematic diagram is low with spinel particles by ferrochrome piece substrate 1
Reflective coating 2 forms.
Fig. 2: at 180 DEG C or 240 DEG C, different mixed solution proportions are lower to react 1 day resulting environment-friendly type antiradar reflectivity membrane material
The XRD diagram of material (see embodiment 1-4).A:180 DEG C of sample, KOH (44.8g), ethyl alcohol (10mL), glycerol (2mL)；Sample b:180
DEG C, KOH (44.8g), ethyl alcohol (15mL), glycerol (2mL)；C:240 DEG C of sample, KOH (44.8g), ethyl alcohol (10mL), glycerol
(2mL)；D:240 DEG C of sample, KOH (44.8g), ethyl alcohol (15mL), glycerol (2mL).As seen from Figure 2, which is point
Spinel structure.
Fig. 3: at 180 DEG C or 240 DEG C, different mixed solution proportions are lower to react 1 day resulting environment-friendly type antiradar reflectivity membrane material
The SEM of material schemes (see embodiment 1-4).A:180 DEG C of sample, KOH (44.8g), ethyl alcohol (10mL), glycerol (2mL)；Sample b:180
DEG C, KOH (44.8g), ethyl alcohol (15mL), glycerol (2mL)；C:240 DEG C of sample, KOH (44.8g), ethyl alcohol (10mL), glycerol
(2mL)；D:240 DEG C of sample, KOH (44.8g), ethyl alcohol (15mL), glycerol (2mL).The material film surface heap as seen from Figure 3
Block has spinelle crystal grain of the size between 0.09~1.9 μm.
Fig. 4: at 180 DEG C or 240 DEG C, different mixed solution proportions are lower to react 1 day resulting environment-friendly type antiradar reflectivity film
The reflectance curve figure of material (see embodiment 1-4).A:180 DEG C of sample, KOH (44.8g), ethyl alcohol (10mL), glycerol (2mL)；
B:180 DEG C of sample, KOH (44.8g), ethyl alcohol (15mL), glycerol (2mL)；C:240 DEG C of sample, KOH (44.8g), ethyl alcohol
(10mL), glycerol (2mL)；D:240 DEG C of sample, KOH (44.8g), ethyl alcohol (15mL), glycerol (2mL).It is anti-to be computed arithmetic average
Rate is penetrated, reflectivity of the sample a to sample d in the section 300~2500nm is respectively 8.98%, 7.25%, 6.73% and 6.01%.
Specific embodiment
Embodiment 1: the preparation of environment-friendly type antiradar reflectivity membrane material:
(1) it will be wiped 20 times with a thickness of the ferrochrome substrate surface of 3mm alcohol swab, keep surface smooth and clean；
(2) reaction solution 80mL is prepared, the specific proportion of reaction solution is: KOH (44.8g), ethyl alcohol (10mL), glycerol
(2mL), remaining is deionized water.Above-mentioned ferrochrome substrate is put into above-mentioned reaction solution, then is added to together anti-
It answers in the liner (100mL) of the polytetrafluoroethylene (PTFE) of kettle, is reacted for 24 hours in 180 degrees Celsius of baking oven；
(3) cooled to room temperature after taking out reaction kettle, then by reaction system ultrasound 1h, then to ultrasonic product into
Row filtering, then filtration product is washed with deionized, last washed product is in 100 DEG C of dryings, gained environment-friendly type antiradar reflectivity
The spinel particles partial size on membrane material surface is at 0.6~1.5 μm.
Obtained environment-friendly type antiradar reflectivity membrane material (is adopted in the arithmetic average reflectivity of 300nm~2500nm spectrum range
With the visible infrared spectrophotometer of near ultraviolet with integrating sphere) it is 8.98%.
Embodiment 2: the preparation of environment-friendly type antiradar reflectivity membrane material:
(1) it will be wiped 20 times with a thickness of the ferrochrome substrate surface of 3mm alcohol swab, keep surface smooth and clean；
(2) reaction solution 80mL is prepared, the specific proportion of reaction solution is: KOH (44.8g), ethyl alcohol (15mL), glycerol
(2mL), remaining is deionized water.Above-mentioned ferrochrome substrate is put into above-mentioned reaction solution, then is added to together anti-
It answers in the liner (100mL) of the polytetrafluoroethylene (PTFE) of kettle, it is lower in 180 degrees Celsius of baking oven to react for 24 hours；
(3) cooled to room temperature after taking out reaction kettle, then by reaction system ultrasound 1h, then to ultrasonic product into
Row filtering, then filtration product is washed with deionized, last washed product is in 100 DEG C of dryings, gained environment-friendly type antiradar reflectivity
The spinel particles partial size on membrane material surface is at 0.4~1.3 μm.
Obtained environment-friendly type antiradar reflectivity membrane material (is adopted in the arithmetic average reflectivity of 300nm~2500nm spectrum range
With the visible infrared spectrophotometer of near ultraviolet with integrating sphere) it is 7.25%.
Embodiment 3: the preparation of environment-friendly type antiradar reflectivity membrane material:
(1) it will be wiped 20 times with a thickness of the ferrochrome substrate surface of 3mm alcohol swab, keep surface smooth and clean；
(2) reaction solution 80mL is prepared, the specific proportion of reaction solution is: KOH (44.8g), ethyl alcohol (10mL), glycerol
(2mL), remaining is deionized water.Above-mentioned ferrochrome substrate is put into above-mentioned reaction solution, then is added to together anti-
It answers in the liner (100mL) of the polytetrafluoroethylene (PTFE) of kettle, it is lower in 240 degrees Celsius of baking oven to react for 24 hours；
(3) cooled to room temperature after taking out reaction kettle, then by reaction system ultrasound 1h, then to ultrasonic product into
Row filtering, then filtration product is washed with deionized, last washed product is in 100 DEG C of dryings, gained environment-friendly type antiradar reflectivity
The spinel particles partial size on membrane material surface is at 0.3~1.39 μm.
Obtained environment-friendly type antiradar reflectivity membrane material (is adopted in the arithmetic average reflectivity of 300nm~2500nm spectrum range
With the visible infrared spectrophotometer of near ultraviolet with integrating sphere) it is 6.73%.
Embodiment 4: the preparation of environment-friendly type antiradar reflectivity membrane material:
(1) it will be wiped 20 times with a thickness of the ferrochrome substrate surface of 3mm alcohol swab, keep surface smooth and clean；
(2) reaction solution 80mL is prepared, the specific proportion of reaction solution is: KOH (44.8g), ethyl alcohol (15mL), glycerol
(2mL), remaining is deionized water.Above-mentioned ferrochrome substrate is put into above-mentioned reaction solution, then is added to together anti-
It answers in the liner (100mL) of the polytetrafluoroethylene (PTFE) of kettle, it is lower in 240 degrees Celsius of baking oven to react for 24 hours；
(3) cooled to room temperature after taking out reaction kettle, then by reaction system ultrasound 1h, then to ultrasonic product into
Row filtering, then filtration product is washed with deionized, last washed product is in 100 DEG C of dryings, gained environment-friendly type antiradar reflectivity
The spinel particles partial size on membrane material surface is at 0.6~0.1 μm.
Obtained environment-friendly type antiradar reflectivity membrane material (is adopted in the arithmetic average reflectivity of 300nm~2500nm spectrum range
With the visible infrared spectrophotometer of near ultraviolet with integrating sphere) it is 6.01%.
Embodiment 5: the preparation of environment-friendly type antiradar reflectivity membrane material:
(1) it will be wiped 20 times with a thickness of the ferrochrome substrate surface of 3mm alcohol swab, keep surface smooth and clean；
(2) reaction solution 80mL is prepared, the specific proportion of reaction solution is: KOH (44.8g), ethyl alcohol (10mL), glycerol
(2mL), remaining is deionized water.Above-mentioned ferrochrome substrate is put into above-mentioned reaction solution, then is added to together anti-
It answers in the liner (100mL) of the polytetrafluoroethylene (PTFE) of kettle, it is lower in 180 degrees Celsius of baking oven to react 10h；
(3) cooled to room temperature after taking out reaction kettle, then by reaction system ultrasound 1h, then to ultrasonic product into
Row filtering, then filtration product is washed with deionized, last washed product is in 100 DEG C of dryings, gained environment-friendly type antiradar reflectivity
The spinel particles partial size on membrane material surface is at 0.7~1.9 μm.
Obtained environment-friendly type antiradar reflectivity membrane material (is adopted in the arithmetic average reflectivity of 300nm~2500nm spectrum range
With the visible infrared spectrophotometer of near ultraviolet with integrating sphere) it is 10.12%.
Embodiment 6: the preparation of environment-friendly type antiradar reflectivity membrane material:
(1) it will be wiped 20 times with a thickness of the ferrochrome substrate surface of 3mm alcohol swab, keep surface smooth and clean；
(2) reaction solution 80mL is prepared, the specific proportion of reaction solution is: KOH (44.8g), ethyl alcohol (10mL), glycerol
(2mL), remaining is deionized water.Above-mentioned ferrochrome substrate is put into above-mentioned reaction solution, then is added to together anti-
It answers in the liner (100mL) of the polytetrafluoroethylene (PTFE) of kettle, it is lower in 240 degrees Celsius of baking oven to react 48h；
(3) cooled to room temperature after taking out reaction kettle, then by reaction system ultrasound 1h, then to ultrasonic product into
Row filtering, then filtration product is washed with deionized, last washed product is in 100 DEG C of dryings, gained environment-friendly type antiradar reflectivity
The spinel particles partial size on membrane material surface is at 0.09~0.7 μm.
Obtained environment-friendly type antiradar reflectivity membrane material (is adopted in the arithmetic average reflectivity of 300nm~2500nm spectrum range
With the visible infrared spectrophotometer of near ultraviolet with integrating sphere) it is 5.91%.
Claims (1)
1. a kind of preparation method of environment-friendly type antiradar reflectivity membrane material, it is characterised in that:
(1) ferrochrome substrate surface is wiped with alcohol swab, keeps surface smooth clean；Ferrochrome substrate presses quality hundred
Score meter, contain Cr, 11%, Fe, 88%, 0 < Cu < 0.1%, 0 < Mn < 0.1%, 0 < Ni < 0.1%, 0 < P < 0.05%, 0 < Mo <
0.1%, 0 < Si < 0.1% and 0 < C < 0.4%, substrate thickness are 0.2~10mm；
(2) substrate is put into 80mL mixed solution, the group of the mixed solution becomes 10~15mL dehydrated alcohol, 1~2mL glycerol
With 22.4g~44.8g KOH, remaining is deionized water；
(3) substrate and mixed solution are fitted into together in the reaction kettle of polytetrafluoroethyllining lining, it is anti-under the conditions of 180~240 DEG C
Answer 10~48h；
(4) it is cooled to room temperature after taking out reaction kettle, then by reaction system 1~12h of ultrasound, then ultrasonic product was carried out
Filter, then filtration product is washed with deionized, last washed product is dried at 30~100 DEG C, to obtain environmental protection
Type antiradar reflectivity membrane material；Spinel particles Fe of the low-reflection film layer by size in 0.09~1.9 μm of section2.58~ 2.59Cr0.28~0.30O4It piles up.
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