CN104005015B - A kind of method of steel surface growth in situ α-Fe2O3 nano-array - Google Patents
A kind of method of steel surface growth in situ α-Fe2O3 nano-array Download PDFInfo
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- CN104005015B CN104005015B CN201410260732.4A CN201410260732A CN104005015B CN 104005015 B CN104005015 B CN 104005015B CN 201410260732 A CN201410260732 A CN 201410260732A CN 104005015 B CN104005015 B CN 104005015B
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Abstract
A kind of steel surface growth in situ α-Fe
2o
3the method of nano-array, it relates to a kind of growth in situ α-Fe
2o
3the method of nano-array.The object of the invention is to solve and existingly on iron plate, prepare α-Fe
2o
3the problem that bonding force is poor, pattern is single and operating process is complicated that nano-array exists.Method: one, carry out polished finish to rectangle iron plate successively, clean and dry, obtains processing rear rectangle iron plate; Two, hydrothermal synthesis reaction, obtains reacting rear iron plate; Three, low-temperature heat treatment, obtains surface in situ growth α-Fe
2o
3the iron plate of nano-array.Advantage: one, overcome the shortcoming that the load of conventional powder synthetic method is difficult, bonding force is poor, iron plate and basic solution can be recycled substantially; Two, the target product that the present invention obtains is evenly distributed, and size tunable, can automatic continuous production on a large scale.The present invention is mainly used at iron plate face growth in situ α-Fe
2o
3nano-array.
Description
Technical field
The present invention relates to a kind of growth in situ α-Fe
2o
3the method of nano-array.
Background technology
In recent years, Fe
2o
3the features such as nano material is cheap due to it, wide material sources obtain and apply more and more widely in gas sensor, organic matter degradation, magneticsubstance, application etc.In addition, because its band gap is 2.2eV, there is the characteristic of n-type semiconductor, also can be applied in the fields such as photocatalysis hydrogen production.
Catalysis and photolysis water all need the α-Fe of loading type
2o
3nano-array is as electrode and medium.α-the Fe of loading type
2o
3the preparation of nano-array mainly adopts the methods such as thermal oxidation method, anodic oxidation, chemical vapour deposition and ald, and general choice FTO, ITO conductive glass etc., as carrier, make α-Fe
2o
3nano-array attachment in its surface.As the people such as XuRui prepare sheet α-Fe by thermal oxidation method on iron foil
2o
3, along with treatment temp and the change of time, its thickness and width change respectively between 10-60nm and 200-800nm, the Fe of the method synthesis
2o
3there is the problem that energy consumption is large, bonding force is poor, and the target product pattern obtained is comparatively single, product purity is not high; The people such as SusantaK successfully prepare α-Fe by anonizing on iron plate
2o
3nanotube, the method uses organic fluoride electrolytic solution, there is the shortcoming that energy consumption is relatively high, growth product morphology is single, stability is not high; Chemical vapour deposition and atomic layer deposition accumulate in that equipment is high, complicated operation, shortcoming consuming time in addition.Existingly in sum on iron plate, prepare α-Fe
2o
3mainly there is the problem that energy consumption is higher, complicated operation, bonding force are poor, preparation technology has certain pollution and product morphology is single in nano-array.
Summary of the invention
The object of the invention is to solve and existingly on iron plate, prepare α-Fe
2o
3the problem that bonding force is poor, pattern is single and operating process is complicated that nano-array exists, provides a kind of steel surface growth in situ α-Fe
2o
3the method of nano-array.
A kind of steel surface growth in situ α-Fe
2o
3the method of nano-array, specifically completes according to the following steps:
One, then pre-treatment: first carry out polished finish to rectangle iron plate is that clean-out system carries out ultrasonic cleaning 10s ~ 60s with dehydrated alcohol, and recycling goes dried up flushing, obtains processing rear rectangle iron plate after naturally drying;
Two, hydrothermal synthesis reaction: rectangle iron plate after process is immersed and is equipped with in the reactor of basic solution, then seal, transfer in air dry oven, hydrothermal synthesis reaction 6h ~ 24h at temperature is 120 ~ 180 DEG C, take out and obtain reacting rear iron plate;
Three, low-temperature heat treatment: with dehydrated alcohol or deionized water for clean-out system cleans iron plate after reaction, retort furnace is put into after drying, with temperature rise rate be 3 DEG C/min ~ 10 DEG C/min is from room temperature to 250 ~ 350 DEG C, and at temperature is 250 ~ 350 DEG C low-temperature heat treatment 1h ~ 5h, obtain surface in situ growth α-Fe
2o
3the iron plate of nano-array.
Advantage of the present invention:
One, the α-Fe for preparing of the present invention
2o
3nano-array is that iron plate growth in situ comes, α-Fe
2o
3the bonding force of nano-array and iron plate is good, macroscopically α-Fe
2o
3nano-array is rendered as redness or bois de rose rete, and the rete adding tensio-active agent can be inclined black, α-Fe on microcosmic
2o
3nano-array shows as the different nanocrystal of pattern, and size, between 50nm ~ 800nm, overcomes the shortcoming that the load of conventional powder synthetic method is difficult, bonding force is poor, and be easy to reclaim, technique is simple, and iron plate and basic solution can be recycled substantially, and consumption is minimum;
Two, the target product that the present invention obtains is evenly distributed, and size tunable, can automatic continuous production on a large scale, and all material and reagent are all very cheap, operate also very simple;
Three, the invention provides a kind of novel process of loaded nano materials synthesis, suitable pre-treating technology is adopted to obtain different surfaces, add template agent or tensio-active agent in the solution, changing the composition of iron plate or adopt other materials as substrate etc., is the preparation of following composite nano materials and the application extension in fields such as photoelectrocatalysiss thereof new approaches.
Four, in fact the present invention provides a kind of hydrothermal method that is easy, cheap, that easily reclaim to prepare pattern to enrich and stable loading type α-Fe
2o
3the method of nano-array: use Fe sheet as matrix, make it provide source of iron; Hydrothermal method is adopted to carry out nano-array preparation; This patent adopts basic solution system, and this point is obviously different from the employing alcoholic solution system of bibliographical information; Whole operation steps only has simple three steps, is respectively pre-treatment, hydro-thermal reaction and low-temperature heat treatment, can full-automatic operation, realizes industrialization scale operation.
The present invention is mainly used at iron plate face growth in situ α-Fe
2o
3nano-array, obtains surface in situ growth α-Fe
2o
3the iron plate of nano-array, the product morphology obtained are various, and be evenly distributed, and particle diameter and large I regulate and control within the specific limits, iron plate and the equal recoverable of solvent, show wide application prospect in fields such as photochemical catalysis, water treatment and gas sensors.
Accompanying drawing explanation
Fig. 1 is the α-Fe that test one obtains
2o
3nano-array scanning electron microscope (SEM) photograph;
Fig. 2 is the α-Fe that test four obtains
2o
3nano-array scanning electron microscope (SEM) photograph;
Fig. 3 is the α-Fe that test five obtains
2o
3nano-array scanning electron microscope (SEM) photograph;
Fig. 4 is the α-Fe that test eight obtains
2o
3nano-array scanning electron microscope (SEM) photograph;
Fig. 5 is α-Fe prepared by test one
2o
3nano-array XRD figure;
Fig. 6 is the surface in situ growth α-Fe that experiment eight obtains
2o
3the Current-potential curve of the iron plate photochemical catalyzing of nano-array.
Embodiment
Embodiment one: present embodiment is a kind of steel surface growth in situ α-Fe
2o
3the method of nano-array, specifically completes according to the following steps:
One, then pre-treatment: first carry out polished finish to rectangle iron plate is that clean-out system carries out ultrasonic cleaning 10s ~ 60s with dehydrated alcohol, and recycling goes dried up flushing, obtains processing rear rectangle iron plate after naturally drying;
Two, hydrothermal synthesis reaction: rectangle iron plate after process is immersed and is equipped with in the reactor of basic solution, then seal, transfer in air dry oven, hydrothermal synthesis reaction 6h ~ 24h at temperature is 120 ~ 180 DEG C, take out and obtain reacting rear iron plate;
Three, low-temperature heat treatment: with dehydrated alcohol or deionized water for clean-out system cleans iron plate after reaction, retort furnace is put into after drying, with temperature rise rate be 3 DEG C/min ~ 10 DEG C/min is from room temperature to 250 ~ 350 DEG C, and at temperature is 250 ~ 350 DEG C low-temperature heat treatment 1h ~ 5h, obtain surface in situ growth α-Fe
2o
3the iron plate of nano-array.
Embodiment two: the difference of present embodiment and embodiment one is: the polished finish described in step one is sand papering, hydrochloric acid system polishing, the chemical rightenning of hydrogen peroxide system, nitric acid system chemical rightenning or electrochemical etching.Other are identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment two is: described sand papering concrete operations are as follows: adopt 800# sand paper 1500# sand paper and 2000# sand paper to polish step by step to rectangle iron plate successively, namely complete sand papering polished finish.Other are identical with embodiment two.
Embodiment four: the difference of present embodiment and embodiment two is: described hydrochloric acid system polishing concrete operations are as follows: first adopt concentration to be that the NaOH aqueous solution of 0.5mol/L ~ 2mol/L carries out oil removal treatment 1min ~ 5min to rectangle iron plate, then the aqueous hydrochloric acid that massfraction is 15% is placed in, and under ultrasonic frequency is 25KHz ~ 40KHz sonochemistry polishing 30s ~ 90s, namely complete hydrochloric acid system polished finish.Other are identical with embodiment two.
Embodiment five: the difference of present embodiment and embodiment two is: described hydrogen peroxide system chemical rightenning concrete operations are as follows: first adopt concentration to be that the NaOH aqueous solution of 0.5mol/L ~ 2mol/L carries out oil removal treatment 1min ~ 5min to rectangle iron plate, carry out rust cleaning 10s ~ 60s with the aqueous hydrochloric acid that massfraction is 5% ~ 15% again, be then placed in H
2o
2in system polishing fluid, and under ultrasonic frequency is 25KHz ~ 40KHz sonochemistry polishing 15s ~ 45s, namely complete hydrogen peroxide system chemical rightenning process; Described H
2o
2system polishing fluid is 30%H by massfraction
2o
2, H
2c
2o
4, urea, additive and deionized water composition, and described H
2o
2in system polishing fluid, massfraction is 30%H
2o
2volumetric concentration be 100mL/L ~ 150mL/L, H
2c
2o
4mass concentration be 60g/L ~ 80g/L, the mass concentration of urea is 15g/L ~ 25g/L, the volumetric concentration of additive is 5mL/L; Wherein said additive is for be mixed by glycerine and the vitriol oil, and the volume ratio of described glycerine and the vitriol oil is 2:3.Other are identical with embodiment two.
Embodiment six: the difference of present embodiment and embodiment two is: described nitric acid system chemical rightenning concrete operations are as follows: first adopt concentration to be that the NaOH aqueous solution of 0.5mol/L ~ 2mol/L carries out oil removal treatment 1min ~ 5min to rectangle iron plate, be then placed in HNO
3in system polishing fluid, and at temperature is 85 ~ 120 DEG C polished finish 10s ~ 20s, namely complete nitric acid system chemical rightenning process; Described HNO
3system polishing fluid is by concentrated nitric acid, the vitriol oil, strong phosphoric acid, CrO
3, additive and deionized water composition, and described HNO
3in system polishing fluid, the volumetric concentration of concentrated nitric acid is 130mL/L ~ 180mL/L, the volumetric concentration of the vitriol oil is 300mL/L ~ 350mL/L, the volumetric concentration of strong phosphoric acid is 400mL/L ~ 550mL/L, CrO
3mass concentration be 8g/L ~ 12g/L, the mass concentration of additive is 1g/L; Wherein said additive is urea.Other are identical with embodiment two.
Embodiment seven: the difference of present embodiment and embodiment two is: described electrochemical etching concrete operations are as follows: first adopt concentration to be that the NaOH aqueous solution of 0.5mol/L ~ 2mol/L carries out oil removal treatment 1min ~ 5min to rectangle iron plate, cleaning with deionized water is placed in electrolyzer again, and arranging current density is 8-30A/dm
2, and at room temperature polished finish 10min ~ 20min, namely complete electrochemical polishing treatment; Described electrochemical polish liquid is made up of the vitriol oil, strong phosphoric acid, oxalic acid, additive and deionized water, and in described electrochemical polish liquid, the volumetric concentration of the vitriol oil is 150mL/L ~ 200mL/L, the volumetric concentration of strong phosphoric acid is 500mL/L ~ 650mL/L, the mass concentration of oxalic acid is 10g/L ~ 15g/L, the mass concentration of additive is 1 ~ 3g/L; Wherein said additive is gelatin.Other are identical with embodiment two.
Embodiment eight: one of present embodiment and embodiment one to seven difference is: the NaOH aqueous solution of to be mass concentration the be 5g/L ~ 50g/L of the basic solution described in step 2, mass concentration are the KOH aqueous solution of 5g/L ~ 50g/L or massfraction is the strong aqua of 28%.Other are identical with embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight difference is: containing tensio-active agent in the basic solution described in step 2, the quality of described tensio-active agent is the thousandth of Solute mass in basic solution; Described tensio-active agent is cetyl trimethylammonium bromide, polyoxyethylene glycol, ammonium persulphate, Sodium dodecylbenzene sulfonate, ammonium phosphate, urea, citrate three sodium, quadrol or polyvinylpyrrolidone.Other are identical with embodiment one to eight.
Adopt following verification experimental verification effect of the present invention
Test one: a kind of steel surface growth in situ α-Fe
2o
3the method of nano-array, specifically completes according to the following steps:
One, pre-treatment: first from thickness be clip 3cm × 2cm rectangle iron plate the Q235 sheet material of 1mm, 800# sand paper 1500# sand paper and 2000# sand paper is adopted to polish step by step to 3cm × 2cm rectangle iron plate more successively, 3cm × 2cm rectangle iron plate after polishing is put into the small beaker ultrasonic cleaning 15s that 10mL dehydrated alcohol is housed, recycling goes dried up flushing, obtains processing rear rectangle iron plate after naturally drying;
Two, hydrothermal synthesis reaction: rectangle iron plate after process is immersed and is equipped with in the teflon-lined reactor of the 30mLNaOH aqueous solution, then seal, transfer in air dry oven, hydrothermal synthesis reaction 12h at temperature is 180 DEG C, take out and obtain reacting rear iron plate; In the NaOH aqueous solution described in step 2, the mass concentration of NaOH is 15g/L;
Three, low-temperature heat treatment: be that clean-out system cleans iron plate after reaction with deionized water, retort furnace is put into after seasoning, with temperature rise rate be 5 DEG C/min from room temperature to 250 DEG C, and at temperature is 250 DEG C low-temperature heat treatment 2h, obtain surface in situ growth α-Fe
2o
3the iron plate of nano-array.
Utilize α-Fe prepared by this test of scanning electron microscopic observation
2o
3nano-array, as shown in Figure 1, Fig. 1 is the α-Fe that test one obtains
2o
3nano-array scanning electron microscope (SEM) photograph, the α-Fe of this test preparation as shown in Figure 1
2o
3nano-array (α type nanometer Fe
2o
3) pattern is square, be uniformly dispersed, size is about 500nm, and with scissors clip one fritter, edge rete does not come off, and iron plate middle body also wrinkle resistant proof bonding force is good.
Utilize the α-Fe that X-ray diffraction analysis instrument is prepared this test
2o
3nano-array is observed, and as shown in Figure 5, Fig. 5 is α-Fe prepared by test one
2o
3nano-array XRD figure, significantly can be observed by Fig. 5 and occur α-Fe at 24 °, 33 °, 35.6 °
2o
3characteristic peak, secondly also there is the diffractive features peak of substrate Fe at 45 °, 65 °, 82 °.
Test two: this test with test a difference be: in step one first from thickness be clip 3cm × 2cm rectangle iron plate the Q235 sheet material of 1mm, employing concentration is that the NaOH aqueous solution of 1mol/L carries out oil removal treatment 3min to 3cm × 2cm rectangle iron plate, then the aqueous hydrochloric acid that massfraction is 15% is placed in, and under ultrasonic frequency is 30KHz sonochemistry polishing 60s, 3cm × 2cm rectangle iron plate after polishing is put into the small beaker ultrasonic cleaning 15s that 10mL dehydrated alcohol is housed, recycling goes dried up flushing, naturally obtain after drying processing rear rectangle iron plate.Other are identical with test one.
Test three: this test with test a difference be: in step one first from thickness be clip 3cm × 2cm rectangle iron plate the Q235 sheet material of 1mm, employing concentration is that the NaOH aqueous solution of 1mol/L carries out oil removal treatment 3min to 3cm × 2cm rectangle iron plate, carry out rust cleaning 30s with the aqueous hydrochloric acid that massfraction is 10% again, be then placed in H
2o
2in system polishing fluid, and under ultrasonic frequency is 30KHz sonochemistry polishing 30s, 3cm × 2cm rectangle iron plate after polishing is put into the small beaker ultrasonic cleaning 15s that 10mL dehydrated alcohol is housed, recycling goes dried up flushing, obtains processing rear rectangle iron plate after naturally drying.Other are identical with test one.
Test four: this test with test a difference be: in step one first from thickness be clip 3cm × 2cm rectangle iron plate the Q235 sheet material of 1mm, first adopt concentration to be that the NaOH aqueous solution of 1mol/L carries out oil removal treatment 3min to 3cm × 2cm rectangle iron plate, be then placed in HNO
3in system polishing fluid, and at temperature is 100 DEG C polished finish 15s, 3cm × 2cm rectangle iron plate after polishing is put into the small beaker ultrasonic cleaning 15s that 10mL dehydrated alcohol is housed, recycling goes dried up flushing, obtains processing rear rectangle iron plate after naturally drying.Other are identical with test one.
Utilize α-Fe prepared by this test of scanning electron microscopic observation
2o
3nano-array, as shown in Figure 2, Fig. 2 is the α-Fe that test four obtains
2o
3nano-array scanning electron microscope (SEM) photograph, the α-Fe of this test preparation as shown in Figure 2
2o
3nano-array (α type nanometer Fe
2o
3) pattern is bar-shaped, be evenly distributed, size is also comparatively homogeneous, and nanorod diameter is between 80nm ~ 100nm, and length has several microns.
Test five: this test with test three differences is: in the NaOH aqueous solution described in step 2, the mass concentration of NaOH is 20g/L, and with the addition of 5mg cetyl trimethylammonium bromide in the described NaOH aqueous solution.Other are identical with test three.
Utilize α-Fe prepared by this test of scanning electron microscopic observation
2o
3nano-array, as shown in Figure 3, Fig. 3 is the α-Fe that test five obtains
2o
3nano-array scanning electron microscope (SEM) photograph, the α-Fe of this test preparation as shown in Figure 3
2o
3nano-array (α type nanometer Fe
2o
3) pattern is the polyhedron that pentagon and hexagon are formed, what be parallel to base plane is regular hexagon, and the length of side is about 600nm.
Test six: this test with test a difference be: in step 2 at temperature is 180 DEG C hydrothermal synthesis reaction 6h.Other are identical with test one.
Test seven: this test with test a difference be: in step 3 with temperature rise rate be 5 DEG C/min from room temperature to 300 DEG C, and at temperature is 300 DEG C low-temperature heat treatment 4h.Other are identical with test one.
Test eight: this test with test three differences is: in the NaOH aqueous solution described in step 2, the mass concentration of NaOH is 20g/L, and with the addition of 5mg ammonium persulphate in the described NaOH aqueous solution.Other are identical with test three.
Utilize α-Fe prepared by this test of scanning electron microscopic observation
2o
3nano-array, as shown in Figure 4, Fig. 4 is the α-Fe that test eight obtains
2o
3nano-array scanning electron microscope (SEM) photograph, the α-Fe of this test preparation as shown in Figure 4
2o
3nano-array (α type nanometer Fe
2o
3) pattern is umbrella shape, there are six faces side, and the length of side is about 400nm.
Test nine: utilize the surface in situ growth α-Fe that electrochemical workstation obtains test eight
2o
3the iron plate of nano-array carries out catalytic performance test, to test the eight surface in situ growth α-Fe obtained
2o
3the iron plate of nano-array, as working electrode, take Ag/AgCl as reference electrode, and supporting electrode adopts platinum filament, and light source is xenon lamp, and electrolytic solution is 1.0mol/LNaOH solution, and as shown in Figure 6, Fig. 6 is the surface in situ growth α-Fe that test eight obtains to test result
2o
3the Current-potential curve of the iron plate photochemical catalyzing of nano-array, in figure, A represents 100mW/cm
2illumination, in figure, B represents unglazed photograph, as shown in Figure 6 in carried out the performance test of photochemical catalyzing, test result shows, after adding illumination, the current density of its catalytic decomposition water is about 0.60mA/cm
2.
Claims (10)
1. a steel surface growth in situ α-Fe
2o
3the method of nano-array, is characterized in that a kind of steel surface growth in situ α-Fe
2o
3the method of nano-array completes according to the following steps:
One, then pre-treatment: first carry out polished finish to rectangle iron plate is that clean-out system carries out ultrasonic cleaning 10s ~ 60s with dehydrated alcohol, and recycling deionized water rinses, and obtains processing rear rectangle iron plate after naturally drying;
Two, hydrothermal synthesis reaction: rectangle iron plate after process is immersed and is equipped with in the reactor of basic solution, then seal, transfer in air dry oven, hydrothermal synthesis reaction 6h ~ 24h at temperature is 120 ~ 180 DEG C, take out and obtain reacting rear iron plate;
Three, low-temperature heat treatment: with dehydrated alcohol or deionized water for clean-out system cleans iron plate after reaction, retort furnace is put into after drying, with temperature rise rate be 3 DEG C/min ~ 10 DEG C/min is from room temperature to 250 ~ 350 DEG C, and at temperature is 250 ~ 350 DEG C low-temperature heat treatment 1h ~ 5h, obtain surface in situ growth α-Fe
2o
3the iron plate of nano-array.
2. a kind of steel surface growth in situ α-Fe according to claim 1
2o
3the method of nano-array, is characterized in that the thickness of the rectangle iron plate described in step one is 1mm.
3. a kind of steel surface growth in situ α-Fe according to claim 1 or 2
2o
3the method of nano-array, is characterized in that the polished finish described in step one is sand papering, hydrochloric acid system polishing, the chemical rightenning of hydrogen peroxide system, nitric acid system chemical rightenning or electrochemical etching.
4. a kind of steel surface growth in situ α-Fe according to claim 3
2o
3the method of nano-array, is characterized in that described sand papering concrete operations are as follows: adopt 800# sand paper, 1500# sand paper and 2000# sand paper to polish step by step to rectangle iron plate successively, namely complete sand papering polished finish.
5. a kind of steel surface growth in situ α-Fe according to claim 3
2o
3the method of nano-array, it is characterized in that described hydrochloric acid system polishing concrete operations are as follows: first adopt concentration to be that the NaOH aqueous solution of 0.5mol/L ~ 2mol/L carries out oil removal treatment 1min ~ 5min to rectangle iron plate, then the aqueous hydrochloric acid that massfraction is 15% is placed in, and under ultrasonic frequency is 25KHz ~ 40KHz sonochemistry polishing 30s ~ 90s, namely complete hydrochloric acid system polished finish.
6. a kind of steel surface growth in situ α-Fe according to claim 3
2o
3the method of nano-array, it is characterized in that described hydrogen peroxide system chemical rightenning concrete operations are as follows: first adopt concentration to be that the NaOH aqueous solution of 0.5mol/L ~ 2mol/L carries out oil removal treatment 1min ~ 5min to rectangle iron plate, carry out rust cleaning 10s ~ 60s with the aqueous hydrochloric acid that massfraction is 5% ~ 15% again, be then placed in H
2o
2in system polishing fluid, and under ultrasonic frequency is 25KHz ~ 40KHz sonochemistry polishing 15s ~ 45s, namely complete hydrogen peroxide system chemical rightenning process; Described H
2o
2system polishing fluid is 30%H by massfraction
2o
2, H
2c
2o
4, urea, additive and deionized water composition, and described H
2o
2in system polishing fluid, massfraction is 30%H
2o
2volumetric concentration be 100mL/L ~ 150mL/L, H
2c
2o
4mass concentration be 60g/L ~ 80g/L, the mass concentration of urea is 15g/L ~ 25g/L, the volumetric concentration of additive is 5mL/L; Wherein said additive is mixed by glycerine and the vitriol oil, and the volume ratio of described glycerine and the vitriol oil is 2:3.
7. a kind of steel surface growth in situ α-Fe according to claim 3
2o
3the method of nano-array, is characterized in that described nitric acid system chemical rightenning concrete operations are as follows: first adopt concentration to be that the NaOH aqueous solution of 0.5mol/L ~ 2mol/L carries out oil removal treatment 1min ~ 5min to rectangle iron plate, be then placed in HNO
3in system polishing fluid, and at temperature is 85 ~ 120 DEG C polished finish 10s ~ 20s, namely complete nitric acid system chemical rightenning process; Described HNO
3system polishing fluid is by concentrated nitric acid, the vitriol oil, strong phosphoric acid, CrO
3, additive and deionized water composition, and described HNO
3in system polishing fluid, the volumetric concentration of concentrated nitric acid is 130mL/L ~ 180mL/L, the volumetric concentration of the vitriol oil is 300mL/L ~ 350mL/L, the volumetric concentration of strong phosphoric acid is 400mL/L ~ 550mL/L, CrO
3mass concentration be 8g/L ~ 12g/L, the mass concentration of additive is 1g/L; Wherein said additive is urea.
8. a kind of steel surface growth in situ α-Fe according to claim 3
2o
3the method of nano-array, it is characterized in that described electrochemical etching concrete operations are as follows: first adopt concentration to be that the NaOH aqueous solution of 0.5mol/L ~ 2mol/L carries out oil removal treatment 1min ~ 5min to rectangle iron plate, cleaning with deionized water is placed in electrolyzer again, and arranging current density is 8-30A/dm
2, and at room temperature polished finish 10min ~ 20min, namely complete electrochemical polishing treatment; Described electrochemical polish liquid is made up of the vitriol oil, strong phosphoric acid, oxalic acid, additive and deionized water, and in described electrochemical polish liquid, the volumetric concentration of the vitriol oil is 150mL/L ~ 200mL/L, the volumetric concentration of strong phosphoric acid is 500mL/L ~ 650mL/L, the mass concentration of oxalic acid is 10g/L ~ 15g/L, the mass concentration of additive is 1 ~ 3g/L; Wherein said additive is gelatin.
9. a kind of steel surface growth in situ α-Fe according to claim 1
2o
3the method of nano-array, is characterized in that the basic solution described in step 2 to be mass concentration is the NaOH aqueous solution of 5g/L ~ 50g/L, the KOH aqueous solution that mass concentration is 5g/L ~ 50g/L or massfraction be the strong aqua of 28%.
10. a kind of steel surface growth in situ α-Fe according to claim 9
2o
3the method of nano-array, is characterized in that the quality of described tensio-active agent is the thousandth of Solute mass in basic solution containing tensio-active agent in the basic solution described in step 2; Described tensio-active agent is cetyl trimethylammonium bromide, polyoxyethylene glycol, ammonium persulphate, Sodium dodecylbenzene sulfonate, ammonium phosphate, urea, trisodium citrate, quadrol or polyvinylpyrrolidone.
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