CN104005015A - Method for conducting in-situ growth of alpha-Fe2O3 nano arrays on surface of steel - Google Patents
Method for conducting in-situ growth of alpha-Fe2O3 nano arrays on surface of steel Download PDFInfo
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- CN104005015A CN104005015A CN201410260732.4A CN201410260732A CN104005015A CN 104005015 A CN104005015 A CN 104005015A CN 201410260732 A CN201410260732 A CN 201410260732A CN 104005015 A CN104005015 A CN 104005015A
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Abstract
The invention relates to a method for conducting in-situ growth of alpha-Fe2O3 nano arrays, in particular to a method for conducting the in-situ growth of the alpha-Fe2O3 nano arrays on the surface of steel. The method aims at solving the problems that when the alpha-Fe2O3 nano arrays are prepared on iron sheets at present, the bonding force is poor, the shape and the appearance are single, and operation procedures are complex. The method includes the steps that (1) polishing processing, washing and airing are sequentially carried out on the rectangular iron sheets, and the processed rectangular iron sheets are obtained; (2) hydro-thermal synthesis reaction is carried out to obtain the iron sheets after reaction; (3) low-temperature heat processing is carried out to obtain the iron sheets with the in-situ growth alpha-Fe2O3 nano arrays on the surfaces. The method has the advantages that the shortcoming that a traditional powder synthesis method is difficult to load and poor in bonding force is overcome, and the iron sheets and alkaline solutions can be basically recycled; a target product obtained with the method is even in distribution, the grain size is adjustable, and large-scale automation continuous production can be achieved. The method is mainly used for conducting the in-situ growth of the alpha-Fe2O3 nano arrays on the surfaces of the iron sheets.
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
3nano material is because it is cheap, and the features such as wide material sources have obtained application more and more widely at aspects such as gas sensor, organic matter degradation, magneticsubstance, applications.In addition, because its band gap is 2.2eV, there is the semi-conductive characteristic of N-shaped, 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 adheres in its surface.As the people such as XuRui prepare sheet α-Fe on iron foil by thermal oxidation method
2o
3, along with the change for the treatment of temp and time, its thickness and width change respectively between 10-60nm and 200-800nm, the Fe that the method is synthetic
2o
3have the problem that energy consumption is large, bonding force is poor, and the target product pattern obtaining is comparatively single, product purity is not high; The people such as Susanta K successfully prepare α-Fe on iron plate by anonizing
2o
3nanotube, the method has been used organic fluoride electrolytic solution, has the shortcoming that energy consumption is relatively high, growth product pattern is single, stability is not high; Chemical vapour deposition and atomic layer deposition accumulate in that equipment is high in addition, complicated operation, shortcoming consuming time.Existing α-the Fe for preparing on iron plate in sum
2o
3nano-array mainly exists that energy consumption is higher, complicated operation, bonding force are poor, preparation technology has certain pollution and the single problem of product pattern.
Summary of the invention
The object of the invention is to solve the existing α-Fe for preparing on iron plate
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, pre-treatment: first rectangle iron plate is carried out to polished finish, then take dehydrated alcohol as clean-out system carries out ultrasonic cleaning 10s～60s, recycle and go dried up flushing, obtain processing rear rectangle iron plate after naturally drying;
Two, hydrothermal synthesis reaction: rectangle iron plate after processing is immersed and is equipped with in the reactor of basic solution, and then sealing, transfers in air dry oven, is hydrothermal synthesis reaction 6h～24h at 120～180 ℃ in temperature, takes out and obtains reacting rear iron plate;
Three, low-temperature heat treatment: take dehydrated alcohol or deionized water cleans reacting rear iron plate as clean-out system, after drying, put into retort furnace, the temperature rise rate of take is warming up to 250～350 ℃ from room temperature as 3 ℃/min～10 ℃/min, and be low-temperature heat treatment 1h～5h at 250～350 ℃ in temperature, obtain surface in situ growth α-Fe
2o
3the iron plate of nano-array.
Advantage of the present invention:
One, α-Fe that prepared by 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, α-Fe in macroscopic view
2o
3nano-array is rendered as redness or bois de rose rete, adds the rete of tensio-active agent can be inclined to one side black, α-Fe on microcosmic
2o
3nano-array shows as the different nanocrystal of pattern, and size, between 50nm～800nm, has overcome conventional powder synthetic method load difficulty, the poor shortcoming of bonding force, 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 particle diameter is controlled, automatic continuous production on a large scale, and all material and reagent are all very cheap, operate also very simple;
Three, the invention provides the synthetic novel process of a kind of loaded nano material, adopt suitable pre-treating technology to obtain different surfaces, in solution, add masterplate agent or tensio-active agent, change the composition of iron plate or adopt other materials as substrate etc., for the preparation of following composite nano materials and at the application extension in the fields such as photoelectrocatalysis new approaches.
Four, in fact the present invention provides a kind of hydrothermal method easy, cheap, that easily reclaim to prepare the abundant and stable loading type α-Fe of pattern
2o
3the method of nano-array: use Fe sheet as matrix, make it that source of iron is provided; Adopt hydrothermal method 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, and realize large-scale industrialization and produce.
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 pattern obtaining are various, be evenly distributed, and particle diameter and large I regulate and control within the specific limits, and the equal recoverable of iron plate and solvent, shows wide application prospect in fields such as photochemical catalysis, water treatment and gas sensors.
Accompanying drawing explanation
Fig. 1 is the test one α-Fe obtaining
2o
3nano-array scanning electron microscope (SEM) photograph;
Fig. 2 is the test four α-Fe that obtain
2o
3nano-array scanning electron microscope (SEM) photograph;
Fig. 3 is the test five α-Fe that obtain
2o
3nano-array scanning electron microscope (SEM) photograph;
Fig. 4 is the test eight α-Fe that obtain
2o
3nano-array scanning electron microscope (SEM) photograph;
Fig. 5 is the α-Fe of test one preparation
2o
3nano-array XRD figure;
Fig. 6 is 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, pre-treatment: first rectangle iron plate is carried out to polished finish, then take dehydrated alcohol as clean-out system carries out ultrasonic cleaning 10s～60s, recycle and go dried up flushing, obtain processing rear rectangle iron plate after naturally drying;
Two, hydrothermal synthesis reaction: rectangle iron plate after processing is immersed and is equipped with in the reactor of basic solution, and then sealing, transfers in air dry oven, is hydrothermal synthesis reaction 6h～24h at 120～180 ℃ in temperature, takes out and obtains reacting rear iron plate;
Three, low-temperature heat treatment: take dehydrated alcohol or deionized water cleans reacting rear iron plate as clean-out system, after drying, put into retort furnace, the temperature rise rate of take is warming up to 250～350 ℃ from room temperature as 3 ℃/min～10 ℃/min, and be low-temperature heat treatment 1h～5h at 250～350 ℃ in temperature, 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 1 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 successively 800# sand paper 1500# sand paper and 2000# sand paper to polish step by step to rectangle iron plate, 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 adopting concentration is that the NaOH aqueous solution of 0.5mol/L～2mol/L carries out oil removal treatment 1min～5min to rectangle iron plate, then be placed in massfraction and be 15% aqueous hydrochloric acid, and be sonochemistry polishing 30s～90s under 25KHz～40KHz in ultrasonic frequency, 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 adopting concentration is that the NaOH aqueous solution of 0.5mol/L～2mol/L carries out oil removal treatment 1min～5min to rectangle iron plate, with the aqueous hydrochloric acid that massfraction is 5%～15% 10s～60s that eliminates rust, be then placed in H again
2o
2in system polishing fluid, and be sonochemistry polishing 15s～45s under 25KHz～40KHz in ultrasonic frequency, complete the chemical rightenning of hydrogen peroxide system and process; Described H
2o
2system polishing fluid is 30%H by massfraction
2o
2, H
2c
2o
4, urea, additive and deionized water form, 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 that the mass concentration of 60g/L～80g/L, urea is that the volumetric concentration of 15g/L～25g/L, additive is 5mL/L; Wherein said additive is for to 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 adopting concentration is that the NaOH aqueous solution of 0.5mol/L～2mol/L carries out oil removal treatment 1min～5min to rectangle iron plate, is then placed in HNO
3in system polishing fluid, and be polished finish 10s～20s at 85～120 ℃ in temperature, complete nitric acid system chemical rightenning and process; Described HNO
3system polishing fluid is by concentrated nitric acid, the vitriol oil, strong phosphoric acid, CrO
3, additive and deionized water form, and described HNO
3in system polishing fluid, the volumetric concentration of concentrated nitric acid is that the volumetric concentration of 130mL/L～180mL/L, the vitriol oil is that the volumetric concentration of 300mL/L～350mL/L, strong phosphoric acid is 400mL/L～550mL/L, CrO
3mass concentration be that the mass concentration of 8g/L～12g/L, 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 adopting concentration is that the NaOH aqueous solution of 0.5mol/L～2mol/L carries out oil removal treatment 1min～5min to rectangle iron plate, with deionized water, clean and be placed in electrolyzer again, it is 8-30A/dm that current density is set
2, and polished finish 10min～20min at room temperature, complete electrochemical polishing treatment; Described electrochemical polish liquid is comprised 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 that the volumetric concentration of 150mL/L～200mL/L, strong phosphoric acid is that the mass concentration of 500mL/L～650mL/L, oxalic acid is that the mass concentration of 10g/L～15g/L, 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 basic solution described in step 2 is that mass concentration is the strong aqua that the NaOH aqueous solution of 5g/L～50g/L, the KOH aqueous solution that mass concentration is 5g/L～50g/L or massfraction are 28%.Other are identical with embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight difference is: contain tensio-active agent in the basic solution described in step 2, the quality of described tensio-active agent is the thousandth of solute quality 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: clip 3cm * 2cm rectangle iron plate the Q235 sheet material that is first 1mm from thickness, adopt successively again 800# sand paper 1500# sand paper and 2000# sand paper to polish step by step to 3cm * 2cm rectangle iron plate, 3cm * 2cm rectangle iron plate after polishing is put into the small beaker ultrasonic cleaning 15s that 10mL dehydrated alcohol is housed, recycling is gone dried up flushing, obtains processing rear rectangle iron plate after naturally drying;
Two, hydrothermal synthesis reaction: rectangle iron plate after processing is immersed and is equipped with in the teflon-lined reactor of the 30mLNaOH aqueous solution, then sealing, transferring in air dry oven, is hydrothermal synthesis reaction 12h at 180 ℃ in temperature, takes out and obtains 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: the deionized water of take cleans reacting rear iron plate as clean-out system, after seasoning, put into retort furnace, the temperature rise rate of take is warming up to 250 ℃ as 5 ℃/min from room temperature, and is low-temperature heat treatment 2h at 250 ℃ in temperature, obtains surface in situ growth α-Fe
2o
3the iron plate of nano-array.
Utilize the α-Fe of this test of scanning electron microscopic observation preparation
2o
3nano-array, as shown in Figure 1, Fig. 1 is the test one α-Fe obtaining
2o
3nano-array scanning electron microscope (SEM) photograph, the as shown in Figure 1 α-Fe of this test preparation
2o
3nano-array (α type nanometer Fe
2o
3) pattern is square shape, is uniformly dispersed, size is 500nm left and right, 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 of X-ray diffraction analysis instrument to this test preparation
2o
3nano-array is observed, and as shown in Figure 5, Fig. 5 is the α-Fe of test one preparation
2o
3nano-array XRD figure, can significantly be observed at 24 °, 33 °, 35.6 ° and occurred α-Fe by Fig. 5
2o
3characteristic peak, secondly at 45 °, 65 °, the 82 ° diffractive features peaks that also occur substrate Fe.
Test two: this test with test one difference is: clip 3cm * 2cm rectangle iron plate the Q235 sheet material that is first 1mm from thickness in step 1, adopt the NaOH aqueous solution that concentration is 1mol/L to carry out oil removal treatment 3min to 3cm * 2cm rectangle iron plate, then be placed in massfraction and be 15% aqueous hydrochloric acid, and be sonochemistry polishing 60s under 30KHz in ultrasonic frequency, 3cm * 2cm rectangle iron plate after polishing is put into the small beaker ultrasonic cleaning 15s that 10mL dehydrated alcohol is housed, recycling is gone dried up flushing, naturally after drying, obtain processing rear rectangle iron plate.Other are identical with test one.
Test three: this test with test one difference is: clip 3cm * 2cm rectangle iron plate the Q235 sheet material that is first 1mm from thickness in step 1, adopt the NaOH aqueous solution that concentration is 1mol/L to carry out oil removal treatment 3min to 3cm * 2cm rectangle iron plate, with the aqueous hydrochloric acid that massfraction is 10% 30s that eliminates rust, be then placed in H again
2o
2in system polishing fluid, and be sonochemistry polishing 30s under 30KHz in ultrasonic frequency, 3cm * 2cm rectangle iron plate after polishing is put into the small beaker ultrasonic cleaning 15s that 10mL dehydrated alcohol is housed, and recycling is gone dried up flushing, obtains processing rear rectangle iron plate after naturally drying.Other are identical with test one.
Test four: this test with test one difference is: clip 3cm * 2cm rectangle iron plate the Q235 sheet material that is first 1mm from thickness in step 1, first adopting concentration is that the NaOH aqueous solution of 1mol/L carries out oil removal treatment 3min to 3cm * 2cm rectangle iron plate, is then placed in HNO
3in system polishing fluid, and be polished finish 15s at 100 ℃ in temperature, 3cm * 2cm rectangle iron plate after polishing is put into the small beaker ultrasonic cleaning 15s that 10mL dehydrated alcohol is housed, and recycling is gone dried up flushing, obtains processing rear rectangle iron plate after naturally drying.Other are identical with test one.
Utilize the α-Fe of this test of scanning electron microscopic observation preparation
2o
3nano-array, as shown in Figure 2, Fig. 2 is the test four α-Fe that obtain
2o
3nano-array scanning electron microscope (SEM) photograph, the as shown in Figure 2 α-Fe of this test preparation
2o
3nano-array (α type nanometer Fe
2o
3) pattern is bar-shaped, is evenly distributed, size is homogeneous comparatively also, and nanometer rod 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 has added 5mg cetyl trimethylammonium bromide in the described NaOH aqueous solution.Other are identical with test three.
Utilize the α-Fe of this test of scanning electron microscopic observation preparation
2o
3nano-array, as shown in Figure 3, Fig. 3 is the test five α-Fe that obtain
2o
3nano-array scanning electron microscope (SEM) photograph, the as shown in Figure 3 α-Fe of this test preparation
2o
3nano-array (α type nanometer Fe
2o
3) pattern is the polyhedron that pentagon and hexagon form, what be parallel to base plane is regular hexagon, the length of side is 600nm left and right.
Test six: this test with test one difference is: be hydrothermal synthesis reaction 6h at 180 ℃ in temperature in step 2.Other are identical with test one.
Test seven: this test with test one difference is: the temperature rise rate of take in step 3 is warming up to 300 ℃ as 5 ℃/min from room temperature, and is low-temperature heat treatment 4h at 300 ℃ in temperature.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 has added 5mg ammonium persulphate in the described NaOH aqueous solution.Other are identical with test three.
Utilize the α-Fe of this test of scanning electron microscopic observation preparation
2o
3nano-array, as shown in Figure 4, Fig. 4 is the test eight α-Fe that obtain
2o
3nano-array scanning electron microscope (SEM) photograph, the as shown in Figure 4 α-Fe of this test preparation
2o
3nano-array (α type nanometer Fe
2o
3) pattern is umbrella shape, there are six faces side, and the length of side is 400nm left and right.
Test nine: utilize electrochemical workstation to testing the eight surface in situ growth α-Fe that obtain
2o
3the iron plate of nano-array carries out catalytic performance test, to test the eight surface in situ growth α-Fe that obtain
2o
3the iron plate of nano-array, as working electrode, be 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 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, adds the current density of its catalytic decomposition water after illumination and 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, pre-treatment: first rectangle iron plate is carried out to polished finish, then take dehydrated alcohol as clean-out system carries out ultrasonic cleaning 10s～60s, recycle and go dried up flushing, obtain processing rear rectangle iron plate after naturally drying;
Two, hydrothermal synthesis reaction: rectangle iron plate after processing is immersed and is equipped with in the reactor of basic solution, and then sealing, transfers in air dry oven, is hydrothermal synthesis reaction 6h～24h at 120～180 ℃ in temperature, takes out and obtains reacting rear iron plate;
Three, low-temperature heat treatment: take dehydrated alcohol or deionized water cleans reacting rear iron plate as clean-out system, after drying, put into retort furnace, the temperature rise rate of take is warming up to 250～350 ℃ from room temperature as 3 ℃/min～10 ℃/min, and be low-temperature heat treatment 1h～5h at 250～350 ℃ in temperature, 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, the thickness that it is characterized in that the rectangle iron plate described in step 1 is 1mm.
3. according to a kind of steel surface growth in situ α-Fe described in claim 1 or 2
2o
3the method of nano-array, is characterized in that the polished finish described in step 1 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 successively 800# sand paper 1500# sand paper and 2000# sand paper to polish step by step to rectangle iron plate, 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 adopting concentration is that the NaOH aqueous solution of 0.5mol/L～2mol/L carries out oil removal treatment 1min～5min to rectangle iron plate, then be placed in massfraction and be 15% aqueous hydrochloric acid, and be sonochemistry polishing 30s～90s under 25KHz～40KHz in ultrasonic frequency, 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 adopting concentration is that the NaOH aqueous solution of 0.5mol/L～2mol/L carries out oil removal treatment 1min～5min to rectangle iron plate, with the aqueous hydrochloric acid that massfraction is 5%～15% 10s～60s that eliminates rust, be then placed in H again
2o
2in system polishing fluid, and be sonochemistry polishing 15s～45s under 25KHz～40KHz in ultrasonic frequency, complete the chemical rightenning of hydrogen peroxide system and process; Described H
2o
2system polishing fluid is 30%H by massfraction
2o
2, H
2c
2o
4, urea, additive and deionized water form, and described H
2o
2in system polishing fluid, massfraction is 30%H
2o
2volumetric concentration be that the mass concentration of 100mL/L～150mL/L, H2C2O4 is that the mass concentration of 60g/L～80g/L, urea is that the volumetric concentration of 15g/L～25g/L, 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 adopting concentration is that the NaOH aqueous solution of 0.5mol/L～2mol/L carries out oil removal treatment 1min～5min to rectangle iron plate, is then placed in HNO
3in system polishing fluid, and be polished finish 10s～20s at 85～120 ℃ in temperature, complete nitric acid system chemical rightenning and process; Described HNO
3system polishing fluid is by concentrated nitric acid, the vitriol oil, strong phosphoric acid, CrO
3, additive and deionized water form, and described HNO
3in system polishing fluid, the volumetric concentration of concentrated nitric acid is that the volumetric concentration of 130mL/L～180mL/L, the vitriol oil is that the volumetric concentration of 300mL/L～350mL/L, strong phosphoric acid is 400mL/L～550mL/L, CrO
3mass concentration be that the mass concentration of 8g/L～12g/L, 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 adopting concentration is that the NaOH aqueous solution of 0.5mol/L～2mol/L carries out oil removal treatment 1min～5min to rectangle iron plate, with deionized water, clean and be placed in electrolyzer again, it is 8-30A/dm that current density is set
2, and polished finish 10min～20min at room temperature, complete electrochemical polishing treatment; Described electrochemical polish liquid is comprised 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 that the volumetric concentration of 150mL/L～200mL/L, strong phosphoric acid is that the mass concentration of 500mL/L～650mL/L, oxalic acid is that the mass concentration of 10g/L～15g/L, 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 is that mass concentration is the strong aqua that the NaOH aqueous solution of 5g/L～50g/L, the KOH aqueous solution that mass concentration is 5g/L～50g/L or massfraction are 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 containing tensio-active agent in the basic solution described in step 2, and the quality of described tensio-active agent is the thousandth of solute quality 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.
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| CN109913893A (en) * | 2019-04-22 | 2019-06-21 | 陕西科技大学 | A kind of ferriferous oxide micron chip self-supporting electrode and its synthetic method |
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| CN110129791A (en) * | 2019-06-10 | 2019-08-16 | 辽宁工程技术大学 | A kind of preparation method of the steel surface composite membrane of resistance to molten aluminum corrosion |
| CN110863211A (en) * | 2019-11-14 | 2020-03-06 | 南通大学 | Electrode for hydrothermal oxidation treatment under alkaline condition and preparation method thereof |
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| CN112928232A (en) * | 2021-01-25 | 2021-06-08 | 燕山大学 | Polyhedral structure iron oxide material and preparation method and application thereof |
| CN112928232B (en) * | 2021-01-25 | 2022-02-08 | 燕山大学 | Polyhedral structure iron oxide material and preparation method and application thereof |
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