CN101285185A - Preparation method of corrosion resistant hydrotalcite-like film at surface of aluminum and aluminum alloy parts - Google Patents
Preparation method of corrosion resistant hydrotalcite-like film at surface of aluminum and aluminum alloy parts Download PDFInfo
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- CN101285185A CN101285185A CNA2008101023804A CN200810102380A CN101285185A CN 101285185 A CN101285185 A CN 101285185A CN A2008101023804 A CNA2008101023804 A CN A2008101023804A CN 200810102380 A CN200810102380 A CN 200810102380A CN 101285185 A CN101285185 A CN 101285185A
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Abstract
The invention relates to a method for preparing erosion resistant hydrotalcite-like films on the surfaces of aluminum and aluminum alloy parts. The method is as follows: firstly, ultrasonic treatment of the metallic aluminum and the aluminum alloy parts is performed respectively in deionized water and acetone so as to remove impurities and oil stains on the surfaces; secondly, the metallic aluminum and the aluminum alloy parts are placed in ammonium salt-bearing soluble divalent metallic salt reaction solution and the parts react with soluble divalent metallic salts in the reaction solution by using the aluminum on the surfaces of the parts as aluminum source, and then the hydrotalcite-like films are synthesized on the surfaces of the parts, wherein, the chemical formula of the film is [M<2+>1-xAl<3+>x (OH) 2]< x+ >.(Y<n->)x/n.mH2O. The technique used by the method is simple; the raw materials are easy to obtain; the cost is low; the repeatability is good; the prepared films have good erosion resistance; and the layered double-hydroxyl composite metal oxide films are possibly used as erosion resistant coatings of the metallic aluminum and the aluminum alloy parts among engineering materials.
Description
Technical field:
Present technique belongs to aluminium and alloy component aseptic technic field thereof, and being specifically related to a kind of surface crystallization method that adopts is the method that matrix prepares hydrotalcite film with aluminium and aluminium alloy part.
Technical background:
Aluminium is usage quantity maximum in the non-ferrous metal, the widest metallic substance of application surface, and range of application is also in continuous expansion.Aluminum material has a series of good physics, chemistry, mechanics and processing characteristics, low as density, plasticity is high, easy reinforcement, conduct electricity, easily reclaim, easily surface treatment etc.Aluminium and aluminium alloy are widely used in fields such as national defense industry, space flight and aviation industry, automobile industry, electronics, instrument and daily goods with its good performance.But the specific activity of aluminium is higher; in the exsiccant atmosphere; though the surface can form oxide membranous layer; matrix there is the certain protection effect; but this oxidation film layer is loose porous; its erosion resistance is relatively poor, thereby presents higher chemically reactive and electrochemical activity, especially all can suffer serious galvanic corrosion in malaria, sulfur-bearing atmosphere and marine atmosphere.The anti-corrosion effect of chromic salt is fine, and technology is more stable, is usually used in the bottom of the anticorrosion and organic coating of aluminium and alloy thereof.Though the chromic salt surface treatment can effectively improve the anticorrosion effect of aluminium and alloy thereof; particularly with after coating combines in the environment of comparatively high temps, to use; but contain hexavalent chromium ion in the chromate treating technology; has toxicity; contaminate environment; and the processing cost height of waste liquid; control, processing and management to the murder by poisoning material relevant with painting process bring serious harm and unnecessary trouble, from nineteen eighty-two the world environments protective tissue just propose restriction and use chromic salt and other to contain chromate compound.The development Chrome-free, effectively, low, the eco-friendly chromic salt of price and inhibiter substitute and the eco-friendly transitional layer treatment process problem that is aeroplane dope solution that industry member presses for, also be the new problem that the scientific worker faces.Therefore, hydrotalcite-based compound is used for the corrosion-resistant field of aluminium and alloy thereof, technology is simple, nontoxic, consuming little energy, economy, fine corrosion resistance, has broad application prospects.
Hydrotalcite-based compound comprises hydrotalcite (Hydrotalcite) and houghite (Hydrotalcite-like compound), its main body generally is made of the oxyhydroxide of two kinds of metals, therefore be called layered di-hydroxyl composite metal oxidate (LayeredDouble Hydroxide is abbreviated as LDH) again.The intercalation compound of LDH is called intercalated houghite.Hydrotalcite, houghite and intercalated houghite are referred to as hydrotalcite intercalation material (LDHs).Such material is a kind of inorganic materials with unique structural characteristics, but has established the basis that this class material might become the corrosion resistant material with potential application foreground as kind characteristics such as modulation in relative broad range of interlayer intercalant anion.
People such as document 1.R.G.Buchheit in Progress in Organic Coating 47 (2003) 174-182 with V
10O
28 6-The zinc-aluminium hydrotalcite-based compound of intercalation and dihydroxy-benzene compounds are mixed to be coated in substrate surface, thinks and suppresses the VO that discharges in the corrosion process
3 -And Zn
2+Substrate there is the certain protection effect.
People such as document 2.Geraint Williams have delivered two pieces of different anions intercalated houghite compounds and have been incorporated among the PVB in Electrochemical and Solid-State Letters, study its provide protection to aluminium alloy.They have proposed intercalant anion and Cl
-Exchange capacity determined the corrosion resistance nature of hydrotalcite-based compound.
In above-mentioned document, the houghite material has corrosion resistance nature preferably as the application of corrosion resistant material.But, mostly adopt powder body material, study to improve the surface filming that is coated in metal substrate after its viscosity itself and organic adhesion agent are mixed, will make the persistence of film be subjected to certain restriction like this, after adding organic compound, its thermostability also can be affected.The hydrotalcite film that we adopt the preparation of surface crystallization method is the corrosion resistant material that directly synthesizes on the surface of aluminium and alloy component thereof as aluminium and alloy component thereof, does not need to add organic adhesion agent, and human body is not had any toxic action and environmentally safe.
Summary of the invention:
The purpose of this invention is to provide the method that a kind of aluminium and aluminium alloy part surface crystallization legal system are equipped with hydrotalcite film.Under the condition that does not add organic adhesion agent, this hydrotalcite film can improve the corrosion resistance nature of aluminium and aluminium alloy part, and the realization preparation process does not have any toxic action and environmentally safe to human body.
The hydrotalcite film that provides among the present invention is to adopt the preparation of surface crystallization method.Utilizing aluminium and alloy component thereof to be matrix, is the aluminium source with the aluminium of parts surface, then synthesis hydrotalcite-like material film in containing bivalent ions solution.The chemical general formula of rete is;
[M
2+ 1-xAl
3+ x(OH)
2]
x+·(Y
n-)
x/n·mH
2O，
M wherein
2+Represent divalent-metal ion Mg
2+, Co
2+, Ni
2+, Ca
2+, Cu
2+, Fe
2+, Mn
2+, Zn
2+In any, that preferable is Zn
2+, Mg
2+, Co
2+, Ni
2+Y
N-Represent the negatively charged ion CO of intercalation
3 2-, NO
3 -, SO
4 2-, Cl
-, F
-Or Br
-In any, that preferable is CO
3 2-, SO
4 2-, NO
3 -Or Cl
-0.2≤x≤0.4,0≤m≤2.
The present invention utilizes the surface crystallization method at aluminium and alloy component surface preparation hydrotalcite film thereof, does not need through anodic oxidation, need be in inert atmosphere, and the deionized water of employing need not remove CO
2, and do not need with adding the corrosion-resistant research that organic tackiness agent can directly apply to aluminium and alloy component thereof.
Concrete preparation method is as follows:
A. aluminium or aluminium alloy part being used deionized water and acetone ultrasonic cleaning 10min respectively, to remove the impurity and the greasy dirt on surface, is 0.1～5% sodium hydroxide solution immersion with massfraction then, removes the zone of oxidation on surface;
B. with solubility ammonium salt (NH
4 +)
nA
N-With solubility divalent metal inorganic salt M
2+B
N-By (NH
4 +)/M
2+Mol ratio is that 2～20 ratio is dissolved in the deionized water, configuration M
2+Concentration of metal ions is the solution of 0.01～1mol/L, and the pH value of regulating this solution with 0.1～3% weak ammonia is 4～10 then;
C. pre-treatment good aluminium or aluminium alloy part are suspended in the reaction soln, reacted 6～120 hours down, take out substrate at 75～180 ℃, at room temperature dry after the ethanolic soln rinsing, promptly obtain hydrotalcite film, the chemical general formula of rete is: [M
2+ 1-xAl
3+ x(OH)
2]
X+(Y
N-)
X/nMH
2O, wherein 0.2≤x≤0.4,0≤m≤2.
A among the step B
N-Be CO
3 2-, NO
3 -, SO
4 2-, Cl
-, F
-Or Br
-In any, that preferable is CO
3 2-, SO
4 2-, NO
3 -Or Cl
-M
2+Being divalent metal, can be Mg
2+, Co
2+, Ni
2+, Ca
2+, Cu
2+, Fe
2+, Mn
2+Or Zn
2+Deng in a kind of, preferably Mg
2+, Co
2+, Zn
2+Or Ni
2+B
N-Be NO
3 -, SO
4 2-, Cl
-, F
-Or Br
-In any, that preferable is SO
4 2-, NO
3 -Or Cl
-(NH
4 +)/M
2+B
N-Mol ratio be 3～10.The preferable pH value scope of reaction soln is 6.0～8.0.
Preferable temperature of reaction is 90～180 ℃ among the step C, and preferable reaction time range is 12～120 hours.
Adopt day island proper Tianjin XRD-6000 type X-ray diffractometer and the German Bruker Vector22 of company type Fourier transformation infrared spectrometer that sample is carried out qualitative analysis, the results are shown in Figure 1.Fig. 1 is hydrotalcite film X-ray diffraction (XRD) collection of illustrative plates that different time obtains among the embodiment 1.Except near the diffraction peak 45 ° and 65 ° is Al
2O
3Diffraction peak outside, other diffraction peak can belong to and is (003) of nitrate radical type hydrotalcite film, (006), (012) diffraction peak.Along with the increase of time, the film diffracted intensity strengthens, and the prolongation along with the reaction times is described, the thickness of film increases.Fig. 2 is the XRD figure spectrum of zinc-aluminum gavite film that obtains among the embodiment 1 and the powder that the zinc-aluminum gavite film is scraped off from the aluminium parts surface.Curve a is the XRD figure spectrum of the zinc-aluminum gavite powder that scrapes off among Fig. 2, and its (003) diffraction peak is the strongest.Curve b is the XRD figure spectrum of zinc-aluminum gavite film among Fig. 2, and its (012) diffraction peak is the strongest, illustrates that the orientation of the zinc-aluminum gavite film that the surface crystallization method prepares is relatively good.
Adopt Japanese HITACHI S-3500N type scanning electronic microscope (SEM) to observe the pattern in film surface and cross section thereof (for more clear all the SEM samples of photograph are all handled through metal spraying).Fig. 3 is the SEM picture of the zinc-aluminum gavite film of preparation among the embodiment 1.Thus picture as can be seen, the hydrotalcite film that aluminium parts surface crystallization method obtains is more even, fine and close.Fig. 4 is the SEM picture in the zinc-aluminum gavite film cross section of preparation among the embodiment 1.Scheme thus as can be seen that the tabular houghite is being closely aligned, and along with the vertical direction growth of substrate.
Adopt the intercalant anion type of German VECTOR22 type Fourier infrared spectrograph detection type hydrotalcite film.Fig. 5 is the FT-IR collection of illustrative plates of the powder that scrapes off of zinc-aluminum gavite film of preparation among the embodiment 1.3450cm
-1The place is the eigen vibration absorption peak of OH, 1628cm
-1The absorption peak at place is H
2The flexural vibration absorption peak of O molecule, 1384cm
-1The absorption peak at place is NO
3 -Vibration absorption peak, illustrate that thus the intercalant anion of the hydrotalcite film of the preparation of surface crystallization method among the embodiment 1 is NO
3 -
Adopt homemade CS300 corrosion electrochemistry mensuration system to measure the polarization curve of aluminium parts and hydrotalcite film sample.Fig. 6 is the aluminium parts of embodiment 1 and the polarization curve of the aluminium parts behind the surface crystallization method synthesis hydrotalcite-like material film, and curve a is the polarization curve of aluminium parts template, and curve b is the polarization curve of the aluminium parts behind the surface crystallization method synthesis hydrotalcite-like material film.As can be seen from Figure, the corrosion current of the aluminium alloy part behind the surface crystallization method synthesis hydrotalcite-like material film obviously reduces, and illustrates that its corrosion resistance nature obviously improves.The polarization curve of the hydrotalcite film of preparation contrast in hydrotalcite film that Fig. 7 obtains for embodiment 1 surface crystallization method and the document 3 (patent application 200610088993.8), curve a is embodiment 1 a synthetic hydrotalcite film curve, curve b is the polarization curve of synthetic hydrotalcite film in the document 3, polarizing current by the hydrotalcite film among the embodiment more as can be seen is littler, illustrates that its corrosion resistance nature is better.
The invention has the beneficial effects as follows: do not need to omit the loaded down with trivial details operation of this step, and need in inert atmosphere, not need to adopt to remove CO through anodic oxidation
2Deionized water, adopt the surface crystallization method successfully to prepare hydrotalcite film, and the hydrotalcite film of the present invention's preparation is dense, corrosion resistance nature is better.The hydrotalcite film of employing surface crystallization method preparation and the bonding force of parts surface are good, do not need to add organic adhesion agent when using as corrosion resistant material, and do not contain poisonous ion in the film, and human body is not had any toxic action and environmentally safe.The used technology of this law is simple, raw material is easy to get, cost is low, good reproducibility, and the film that makes has the superior corrosion resistance energy, and this hydrotalcite film is expected to use as aluminium in the engineering materials and alloy component corrosion-resistant finishes thereof.
Description of drawings:
The XRD of the hydrotalcite film of the different time that Fig. 1 obtains for embodiment 1;
The XRD of hydrotalcite film that Fig. 2 obtains for embodiment 1 and the powder that scrapes off from the aluminium parts surface;
The SEM of the hydrotalcite film that Fig. 3 obtains for embodiment 1;
The SEM in the hydrotalcite film cross section that Fig. 4 obtains for embodiment 1;
The FT-IR of the powder that the hydrotalcite film that Fig. 5 obtains for embodiment 1 scrapes off;
Aluminium parts that Fig. 6 obtains for embodiment 1 and surface crystallization legal system are equipped with the polarization curve of the aluminium parts behind the hydrotalcite film;
The polarization curve of the hydrotalcite film of the method preparation of hydrotalcite film that Fig. 7 obtains for embodiment 1 and employing document 3.
Specific embodiments:
Below the present invention is further described in conjunction with specific examples:
Embodiment 1:
A. the pre-treatment of aluminium parts: aluminium parts is used deionized water and acetone ultrasonic cleaning 10min respectively, to remove the impurity and the greasy dirt on surface, is 0.5% sodium hydroxide solution immersion with massfraction then, removes the zone of oxidation on surface;
B. take by weighing zinc nitrate 0.595g, ammonium nitrate 0.96g, dissolve in the 200ml deionized water, preparation NH
4 +: Zn
2+Mol ratio is 6 reaction soln 200ml, wherein Zn
2+Volumetric molar concentration be 0.01mol/L, regulate pH to 6.5 with 1% ammoniacal liquor;
C. pre-treatment is good aluminium parts is hung in the reaction soln, places 24h for 120 ℃.Afterwards, after taking out substrate and cleaning with ethanol, seasoning obtains the surface, and to be covered with interlayer anion be NO
3 -The aluminium parts of zinc-aluminum gavite film, the molecular formula of this hydrotalcite film is [Zn
2+ 1-xAl
3+ x(OH)
2]
X+(NO
3 -)
X/nMH
2O.
Embodiment 2:
A. the pre-treatment of aluminium parts: aluminium parts is used deionized water and acetone ultrasonic cleaning 10min respectively, to remove the impurity and the greasy dirt on surface, is 0.5% sodium hydroxide solution immersion with massfraction then, removes the zone of oxidation on surface;
B. take by weighing nickelous nitrate 1.745g, ammonium nitrate 2.881g, dissolve in the 200ml deionized water, preparation NH
4 +: Ni
2+Mol ratio is 6 reaction soln 200ml, wherein Ni
2+Volumetric molar concentration be 0.03mol/L, regulate pH to 7.5 with 0.5% ammoniacal liquor;
C. pre-treatment is good aluminium parts is hung in the reaction soln, places 24h for 150 ℃.Afterwards, take out after the back cleans with ethanol, seasoning obtains the surface, and to be covered with interlayer anion be NO
3 -The aluminium parts of nickel aluminium hydrotalcite film, the molecular formula of this hydrotalcite film is [Ni
2+ 1-xAl
3+ x(OH)
2]
X+(NO
3 -)
X/nMH
2O.
Embodiment 3:
A. the pre-treatment of aluminium parts: aluminium parts is used deionized water and acetone ultrasonic cleaning 10min respectively, to remove the impurity and the greasy dirt on surface, is 1.0% sodium hydroxide solution immersion with massfraction then, removes the zone of oxidation on surface;
B. take by weighing zinc chloride 27.232g, ammonium chloride 32.094g, dissolve in the 200ml deionized water, preparation NH
4 +: Zn
2+Mol ratio is 4 reaction soln 200ml, wherein Zn
2+Volumetric molar concentration be 1.0mol/L, regulate pH to 7.0 with 0.1% dilute ammonia solution;
C. pre-treatment is good aluminium parts is hung in the reaction soln, places 36h for 90 ℃.Afterwards, take out after the back cleans with ethanol, seasoning obtains the surface, and to be covered with interlayer anion be Cl
-The aluminium parts of zinc-aluminum gavite film, the molecular formula of this hydrotalcite film is [Zn
2+ 1-xAl
3+ x(OH)
2]
X+(Cl
-)
X/nMH
2O.
Embodiment 4:
A. the pre-treatment of aluminium parts: aluminium parts is used deionized water and acetone ultrasonic cleaning 10min respectively, to remove the impurity and the greasy dirt on surface, is 1.0% sodium hydroxide solution immersion with massfraction, to remove the zone of oxidation on surface then;
B. take by weighing zinc sulfate 0.323g, ammonium sulfate 2.642g, dissolve in the 200ml deionized water, preparation NH
4 +: Zn
2+Mol ratio is 10 reaction soln 200ml, wherein Zn
2+Volumetric molar concentration be 0.01mol/L, be that 2% ammonia soln is regulated pH to 6.0 with concentration;
C. pre-treatment is good aluminium parts is hung in the reaction soln, places 12h for 180 ℃.Afterwards, take out after the back cleans with ethanol, seasoning obtains the surface, and to be covered with intercalant anion be SO
4 2-The aluminium parts of zinc-aluminum gavite film, the molecular formula of this hydrotalcite film is [Zn
2+ 1-xAl
3+ x(OH)
2]
X+(SO
4 2-)
X/nMH
2O.
Embodiment 5:
A. the pre-treatment of aluminium alloy part: aluminium alloy part is used deionized water and acetone ultrasonic cleaning 10min respectively, to remove the impurity and the greasy dirt on surface, is 3.0% sodium hydroxide solution immersion with massfraction then, removes the zone of oxidation on surface;
B. take by weighing zinc nitrate 0.595g, ammonium nitrate 2.40g, dissolve in the 200ml deionized water, preparation NH
4 +: Zn
2+Mol ratio is 15 reaction soln 200ml, wherein Zn
2+Volumetric molar concentration be 0.01mol/L, be that 3% ammonia soln is regulated pH to 5.5 with concentration;
C. pre-treatment is good aluminium alloy part is hung in the reaction soln, places after the 24h for 150 ℃, takes out after the back cleans with ethanol, and seasoning obtains the surface, and to be covered with intercalant anion be NO
3 -The aluminium alloy part of zinc-aluminum gavite film, the molecular formula of this hydrotalcite film is [Zn
2+ 1-xAl
3+ x(OH)
2]
X+(NO
3 -)
X/nMH
2O.
Embodiment 6:
A. the pre-treatment of aluminium alloy part: aluminium alloy part is used deionized water and acetone ultrasonic cleaning 10min respectively, to remove the impurity and the greasy dirt on surface, is 3.0% sodium hydroxide solution immersion with massfraction, to remove the zone of oxidation on surface then;
B. take by weighing nickelous nitrate 5.816g, ammonium nitrate 12.806g, dissolve in the 200ml deionized water, preparation NH
4 +: Ni
2+Mol ratio is 8 reaction soln 200ml, wherein Ni
2+Volumetric molar concentration be 0.1mol/L, be that 1.5% ammoniacal liquor is regulated pH to 7.5 with concentration;
C. pre-treatment is good aluminium alloy part is hung in the reaction soln, places after the 36h for 120 ℃, takes out after the back cleans with ethanol, and seasoning obtains the surface, and to be covered with intercalant anion be NO
3 -The aluminium alloy part of nickel aluminium hydrotalcite film, the molecular formula of this hydrotalcite film is [Ni
2+ 1-xAl
3+ x(OH)
2]
X+(NO
3 -)
X/nMH
2O.
Claims (4)
1. the preparation method of aluminium and alloy component thereof surface erosion resistance hydrotalcite film, concrete steps are:
A. aluminium or aluminium alloy part being used deionized water and acetone ultrasonic cleaning 10min respectively, to remove the impurity and the greasy dirt on surface, is 0.1～5% sodium hydroxide solution immersion with massfraction then, removes the zone of oxidation on surface;
B. with solubility ammonium salt (NH
4 +)
nA
N-With solubility divalent metal inorganic salt M
2+B
N-By (NH
4 +)/M
2+Mol ratio be that 2～20 ratio is dissolved in the deionized water, configuration M
2+Concentration of metal ions is the reaction soln of 0.01～1mol/L, and the pH value of regulating this solution with 0.1～3% weak ammonia is 4～10 then;
C. pre-treatment good aluminium or aluminium alloy part are suspended in the reaction soln, reacted 6～120 hours down, take out substrate at 75～180 ℃, at room temperature dry after the ethanolic soln rinsing, promptly obtain hydrotalcite film, the chemical general formula of rete is: [M
2+ 1-xAl
3+ x(OH)
2]
X+(Y
N-)
X/nMH
2O, wherein 0.2≤x≤0.4,0≤m≤2;
A among the step B
N-Be CO
3 2-, NO
3 -, SO
4 2-, Cl
-, F
-Or Br
-In any; B
N-Be NO
3 -, SO
4 2-, Cl
-, F
-Or Br
-In any;
M described in step B and the C
2+Represent divalent-metal ion Mg
2+, Co
2+, Ni
2+, Ca
2+, Cu
2+, Fe
2+, Mn
2+, Zn
2+In any; The described Y of step C
N-Represent the negatively charged ion CO of intercalation
3 2-, NO
3 -, SO
4 2-, Cl
-, F
-Or Br
-In any.
2. the preparation method of aluminium according to claim 1 and alloy component surface erosion resistance hydrotalcite film thereof is characterized in that (NH among the step B
4 +)/M
2+Mol ratio be 3～10, with pH value to 6.0～8.0 of weak ammonia conditioned reaction solution; The temperature of reaction of parts in reaction soln is 90～180 ℃ among the step C, and the reaction times is 12～120 hours.
3. the preparation method of aluminium according to claim 1 and alloy component surface erosion resistance hydrotalcite film thereof is characterized in that A among the step B
N-Be CO
3 2-, SO
4 2-, NO
3 -Or Cl
-Bn
-Be SO
4 2-, NO
3 -Or Cl
-
4. the preparation method of aluminium according to claim 1 and alloy component surface erosion resistance hydrotalcite film thereof is characterized in that the M described in the step C
2+Be Zn
2+, Mg
2+, Co
2+Or Ni
2+, Y
N-Be CO
3 2-, SO
4 2-, NO
3 -Or Cl
-
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| CN102343283A (en) * | 2011-07-21 | 2012-02-08 | 北京化工大学 | Vertically aligned layered double hydroxides (LDHs) film and application thereof in structured catalysis |
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| CN102343283A (en) * | 2011-07-21 | 2012-02-08 | 北京化工大学 | Vertically aligned layered double hydroxides (LDHs) film and application thereof in structured catalysis |
| CN102343283B (en) * | 2011-07-21 | 2013-07-17 | 北京化工大学 | Vertically aligned layered double hydroxides (LDHs) film and application thereof in structured catalysis |
| WO2013021368A1 (en) | 2011-08-11 | 2013-02-14 | Universidade De Aveiro | Conversion films based on lamellar double-hydroxides for active protection against corrosion |
| CN102489301A (en) * | 2011-11-24 | 2012-06-13 | 北京化工大学 | Structured copper-cobalt based catalyst and application of catalytic synthesis gas of structured copper-cobalt based catalyst in preparation of higher alcohols |
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| CN106868483A (en) * | 2017-02-28 | 2017-06-20 | 北京石油化工学院 | A kind of preparation method of aluminium and aluminum alloy surface ternary houghite film |
| CN109852992A (en) * | 2019-01-25 | 2019-06-07 | 浙江大学 | Water nano-chip arrays electrode and its preparation method and application is decomposed in a kind of efficient electro-catalysis entirely |
| CN110711553A (en) * | 2019-11-20 | 2020-01-21 | 广州大学 | Hydrotalcite-pseudo-boehmite composite film and preparation method and application thereof |
| CN111733411A (en) * | 2020-07-06 | 2020-10-02 | 北京石油化工学院 | Metal organic framework compound corrosion-resistant film and preparation method thereof |
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