CN108707941B - Anodic oxide film, preparation method thereof, aluminum alloy shell containing anodic oxide film and mobile phone - Google Patents
Anodic oxide film, preparation method thereof, aluminum alloy shell containing anodic oxide film and mobile phone Download PDFInfo
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- CN108707941B CN108707941B CN201810533865.2A CN201810533865A CN108707941B CN 108707941 B CN108707941 B CN 108707941B CN 201810533865 A CN201810533865 A CN 201810533865A CN 108707941 B CN108707941 B CN 108707941B
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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- H—ELECTRICITY
- H04—ELECTRIC COMMUNICATION TECHNIQUE
- H04M—TELEPHONIC COMMUNICATION
- H04M1/00—Substation equipment, e.g. for use by subscribers
- H04M1/02—Constructional features of telephone sets
- H04M1/0202—Portable telephone sets, e.g. cordless phones, mobile phones or bar type handsets
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Abstract
The invention discloses an anodic oxide film, a preparation method thereof, an aluminum alloy shell containing the anodic oxide film and a mobile phone. The preparation method comprises the following steps: carrying out anodic oxidation and hole sealing treatment on the aluminum alloy shell; the thickness of the side wall of the aluminum alloy shell is more than or equal to 0.85mm, and the smooth transition of the aluminum alloy shell in the thickness direction is more than or equal to 1: 20; the anodic oxidation conditions are as follows: the oxidation voltage is 11.5V-15V, and the current density is 1.2-2A/dm2The concentration of the electrolyte is 180-200 g/L; the conditions of the hole sealing treatment are as follows: the concentration of the hole sealing liquid is 12-15 g/L; the thickness of the anodic oxide film is more than 15 μm. The density of the anode oxide film of the aluminum alloy shell prepared by the invention is more than 0.6, the hardness reaches more than 100HB, and alpha-Al2O3The content is more than 80 percent, and the 'sliding layer' of the anode film in the falling process can be effectively reduced.
Description
Technical Field
The invention relates to an anodic oxide film, a preparation method thereof, an aluminum alloy shell containing the anodic oxide film and a mobile phone.
Background
In recent years, with the continuous innovation of the smart mobile phone technology, the differentiation competition among mobile phone manufacturers becomes more and more severe, and various products with great innovation emerge, wherein the smart mobile phone with a metal body is a breakthrough in the field of mobile phone structural members. For a mobile phone, the appearance is often the most important part for consumers, and the material is an important aspect for determining the appearance of the mobile phone, and the model of the metal body design has excellent texture and is more and more favored by consumers. Currently, the mainstream metal machine types on the market represent OPPO R9s, OPPO R9, HTC ONE M9, Huaqi P8, iPhone6 and the like.
The mobile phone with the metal shell can show excellent texture and gorgeous target color, and the surface of the aluminum alloy which is taken as the raw material of the current mainstream body structural part is subjected to anodic treatment, so that the mobile phone has the performances of rich color, beautiful color, good insulation, hardness, wear resistance and extremely high corrosion resistance.
Due to the shielding property of the aluminum alloy material to radio frequency signals, the thickness of the aluminum alloy shell is required to be reduced to the maximum extent (the maximum large surface thickness is 0.60mm, and the local thickness is 0.50mm) when a mobile phone is designed. However, the thinner thickness will lead to the irreversible deformation of the aluminum alloy to lead the anode film to deform and crack when the stress σ is larger than σ e in the process of drop test, and the unrecoverable damage of the appearance of the mobile phone will bring serious negative effects to the experience of consumers.
Disclosure of Invention
The invention aims to solve the technical problem that an anodic oxide film cracks in the falling process of an aluminum alloy shell of a mobile phone, and simultaneously meets the antenna performance of the mobile phone, and simultaneously ensures the stable adhesion of the shell structure and the anodic oxide film, thereby providing the anodic oxide film, the preparation method thereof, the aluminum alloy shell containing the anodic oxide film and the mobile phone. The density of the anode oxide film of the aluminum alloy shell prepared by the invention is more than 0.6, the hardness reaches more than 100HB, and alpha-Al2O3The content is more than 80%, so that a 'sliding layer' of the anode film in the falling process can be effectively reduced, the adhesive force of the anode oxide film is stable, and the deformation rate of the shell in the falling process is greatly reduced.
The invention provides a preparation method of an anodic oxide film of an aluminum alloy shell, which comprises the following steps of carrying out anodic oxidation and hole sealing treatment on the aluminum alloy shell;
the thickness of the side wall of the aluminum alloy shell is more than or equal to 0.85mm, and the smooth transition of the aluminum alloy shell in the thickness direction is more than or equal to 1: 20;
the anodic oxidation conditions are as follows: the oxidation voltage is 11.5V-15V, and the current density is 1.2-2A/dm2The concentration of the electrolyte is 180-200 g/L;
the hole sealing treatment conditions are as follows: the concentration of the hole sealing liquid is 12-15 g/L;
the thickness of the anodic oxide film is more than 15 μm.
In the invention, the smooth transition of the aluminum alloy shell in the thickness direction is more than or equal to 1:20, which means that the tangent value of an included angle formed by the aluminum alloy shell in the thickness direction is more than or equal to 1: 20.
In the present invention, the oxidation voltage is preferably 11.5 to 12.5V, for example, 11.5V or 12.5V. The compactness of the anodic oxide film in the oxidation voltage range is improved by 12% compared with that of the anodic oxide film with the voltage of 9.0-11.5V.
In the present invention, the current density is preferably 1.2 to 1.5A/dm2For example 1.2A/dm2、1.5A/dm2。
In the present invention, the thickness of the anodic oxide film is preferably 15 to 18 μm.
In the present invention, the electrolyte may be an electrolyte conventional in the art, and is preferably a chemical polishing mixed acid. The chemical polishing mixed acid can be commonly available or obtained by conventional methods, for example, the chemical polishing mixed acid is purchased from Shenzhen Shenyuan Ganjiang chemical industry Co.
In the present invention, the electrolyte concentration generally refers to the mass-to-volume ratio of all solutes to the solvent in the electrolyte, and is preferably 200 g/L.
In the invention, the temperature of the electrolyte is preferably 18-21 ℃, the thickness of the anode film is uniform in the temperature range, and the thickness can be controlled within 1 μm. The anode film is uniform, so that the problem of 'sliding layer' of the anode film in the falling process can be reduced.
In the present invention, the time for the anodic oxidation may be an oxidation time conventional in the art, and is preferably 30 min.
In the invention, the pore sealing liquid can be commonly sold in the market or obtained by a conventional method, for example, the pore sealing liquid is purchased from a Shenzhen Shanghai Source fine chemical processing plant.
In the invention, the concentration of the hole sealing liquid generally refers to the mass-volume ratio of all solutes to a solvent in the hole sealing liquid, preferably 13-14 g/L, and the hardness of the anodic oxide film can reach more than 100HB under the concentration of the hole sealing liquid.
In the invention, the time of the hole sealing treatment is preferably 15-20 min.
In the invention, the temperature of the hole sealing treatment is preferably 80-85 ℃.
As is known to those skilled in the art, the anodization is generally carried out in an electrolytic cell, and preferably, the frequency of the change of deionized water in the electrolytic cell in the anodization is 24 hours or less.
In the invention, preferably, before the anodic oxidation, the aluminum alloy shell is washed by deionized water with conductivity less than or equal to 35 us/cm.
In the present invention, preferably, the aluminum alloy case is cleaned after the anodic oxidation; more preferably, the aluminum alloy housing is rinsed with deionized water after anodization.
In a preferred embodiment of the present invention, the oxidation voltage is 11.5 to 12.5V, and the current density is 1.2 to 1.5A/dm2The concentration of the electrolyte is 180-200 g/L, and the concentration of the hole sealing liquid is 13-14 g/L.
In a preferred embodiment of the present invention, the oxidation voltage is 11.5V, and the current density is 1.2A/dm2The concentration of the electrolyte is 200g/L, and the concentration of the hole sealing liquid is 13 g/L.
In a preferred embodiment of the present invention, the oxidation voltage is 12.5V, and the current density is 1.5A/dm2The concentration of the electrolyte is 200g/L, and the concentration of the hole sealing liquid is 14 g/L.
In a preferred embodiment of the present invention, the oxidation voltage is 13.5V, and the current density is 1.8A/dm2The concentration of the electrolyte is 180g/L, and the concentration of the hole sealing liquid is 12 g/L.
In a preferred embodiment of the present invention, the oxidation voltage is 15V and the current density is 2A/dm2The concentration of the electrolyte is 180g/L, and the concentration of the hole sealing liquid is 15 g/L.
The invention also provides the anodic oxide film prepared by the preparation method.
Wherein the density of the anodized film is preferably 0.6 or more. The compactness refers to the volume percentage of atoms in a unit cell, namely the ratio of the volume of atoms contained in the unit cell to the volume of the unit cell.
The hardness of the anodic oxide film is preferably 100HB or more.
Wherein the composition of the anodic oxide film is preferably alpha-Al2O3The content is more than 80 percent, and the percentage refers to alpha-Al in the anodic oxide film2O3The mass percentage of the composite material is calculated.
The invention also provides an aluminum alloy shell containing the anodic oxide film.
The invention also provides a mobile phone comprising the aluminum alloy shell.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
(1) the thickness of the anode oxide film of the aluminum alloy shell prepared by the invention is more than 15 mu m, the density is more than 0.6, the hardness reaches more than 100HB, and the alpha-Al2O3The content is more than 80%, so that a 'sliding layer' of the anode film in the falling process can be effectively reduced, the adhesive force of the anode oxide film is stable, and the shell deformation rate and the anode film cracking rate in the falling process are greatly reduced.
(2) According to the invention, the thickness of the side wall of the aluminum alloy shell is more than or equal to 0.85mm, on the basis of the thickness, the antenna performance can be adjusted and satisfied, the structural strength can be ensured, and the shell deformation in the falling process can be reduced.
(3) The aluminum alloy shell of the mobile phone containing the anodic oxide film prepared by the invention has smooth transition in the thickness direction of more than or equal to 1:20, and can effectively avoid the deformation of the shell and the tearing of the anodic film caused by the concentration of drop stress.
(4) In the invention, after the aluminum alloy shell of the mobile phone is anodized, the body of the mobile phone has beautiful color, good insulation, hardness, wear resistance and good corrosion resistance.
Drawings
Fig. 1 is a schematic structural view of an aluminum alloy shell in the thickness direction, wherein a is a schematic structural view of an aluminum alloy shell in the thickness direction in the prior art, and an arrow indicates that an included angle formed by the aluminum alloy shell in the thickness direction is 90 °; b, a diagram is a structural schematic diagram of the aluminum alloy shell in the thickness direction in the embodiments 1-4, an arrow point refers to an included angle formed by the aluminum alloy shell in the thickness direction, and a tangent value of the included angle, namely a line segment (i): the value of the line segment II is more than or equal to 1: 20;
FIG. 2 is a schematic view showing the cracking of an anodic oxide film of a mobile phone; wherein the c picture is a global picture of the anodic oxide film cracking; the figure a and the figure b are partial enlarged views; wherein the image a is taken perpendicular to the plane of the oxide film and the image b is taken at 45 DEG to the plane of the oxide film.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
FIG. 1 is a schematic structural view in the thickness direction of an aluminum alloy shell; wherein, a is a structural schematic diagram of the aluminum alloy shell in the thickness direction in the prior art, and an arrow indicates that an included angle formed by the aluminum alloy shell in the thickness direction is 90 degrees; b, a diagram is a structural schematic diagram of the aluminum alloy shell in the thickness direction in the embodiments 1-4, an arrow point refers to an included angle formed by the aluminum alloy shell in the thickness direction, and a tangent value of the included angle, namely a line segment (i): the value of the line segment II is more than or equal to 1: 20.
In the following examples, the mold of the aluminum alloy case used is shown in b of fig. 1.
Example 1
(1) The polishing machine uses different types of abrasive paper to polish the aluminum alloy shell from coarse to fine, the thickness of the side wall of the aluminum alloy shell is more than or equal to 0.85mm, and the smooth transition in the thickness direction is more than or equal to 1: 20.
(2) Washing the aluminum alloy shell with deionized water, then soaking the aluminum alloy in an oil removing solution (P3Almeco 36) for 10min at 65 ℃; washing the aluminum alloy with deionized water, soaking the aluminum sheet in strong alkaline solution (TURCO aluminum) at 60 deg.C for 2 min; washing the aluminum substrate with deionized water, placing in acid solution (TURCO Liquid Smut Go NC), and soaking at 50 deg.C for 10 min; and (4) washing the aluminum substrate by deionized water with the conductivity of less than or equal to 35us/cm to obtain the pretreated aluminum alloy shell.
(3) The electrolyte is a mixed solution of concentrated sulfuric acid and tartaric acid (purchased from Shenzhen Xin Yuan Ganji Co., Ltd.), the concentration of the electrolyte is 200g/L, the pretreated aluminum alloy shell is used as an anode, the cathode is pure aluminum, and a power supply is connected to prepare an anodic oxide film(ii) a The temperature of the bath solution is 18 ℃, the oxidation voltage is 11.5V, and the current density is 1.2A/dm2The oxidation time was 30 min. The deionized water in the electrolytic cell was replaced once every 24 hours.
(4) And (4) sealing the aluminum alloy shell subjected to anodic oxidation in the step (3), wherein the concentration of the sealing liquid is 13g/L, and sealing the hole for 15-20 min at 80-85 ℃ by using the sealing liquid (purchased from Shenzhen Hai Tong Source fine chemical processing factory).
The thickness of the anodic oxide film of the aluminum alloy shell prepared by the embodiment is 18 mu m, the compactness is more than 0.70, the hardness of the oxide film is more than 100HB, and alpha-Al in the anodic oxide film2O3The content is 85%.
Example 2
The preparation conditions for preparing the anodic oxide film in the step (3) are as follows: the electrolyte concentration is 200g/L, the bath solution temperature is 19 ℃, the oxidation voltage is 12.5V, and the current density is 1.5A/dm2. The concentration of the hole sealing liquid in the step (4) is 14 g/L. The other operations and conditions were the same as in example 1.
The thickness of the anodic oxide film of the aluminum alloy shell prepared by the embodiment is 18 μm, the compactness is more than 0.80, and the hardness of the oxide film is more than 100 HB. alpha-Al in anodic oxide films2O3The content is 80%.
Example 3
The preparation conditions for preparing the anodic oxide film in the step (3) are as follows: the electrolyte concentration is 180g/L, the bath solution temperature is 20 ℃, the oxidation voltage is 13.5V, and the current density is 1.8A/dm2. The concentration of the hole sealing liquid in the step (4) is 12 g/L. The other operations and conditions were the same as in example 1.
The thickness of the anodic oxide film of the aluminum alloy shell prepared by the embodiment is more than 15 μm, the compactness is more than 0.6, and the hardness of the oxide film is more than 100 HB. alpha-Al in anodic oxide films2O3The content is more than 80%.
Example 4
The preparation conditions for preparing the anodic oxide film in the step (3) are as follows: the concentration of the electrolyte is 180g/L, the temperature of the bath solution is 21 ℃, the oxidation voltage is 15V, and the current density is 2A/dm2. The concentration of the hole sealing liquid in the step (4) is 15 g/L. The rest of the operation and conditions were the same as those in the examples1。
The thickness of the anodic oxide film of the aluminum alloy shell prepared by the embodiment is more than 15 μm, the compactness is more than 0.6, and the hardness of the oxide film is more than 100 HB. alpha-Al in anodic oxide films2O3The content is more than 80%.
Comparative example 1
The preparation conditions for preparing the anodic oxide film in the step (3) are as follows: the temperature of the bath solution is 25 ℃, the oxidation voltage is 9V, and the current density is 1.5A/dm2. The concentration of the hole sealing liquid in the step (4) is 10 g/L. The other operations and conditions were the same as in example 1.
The thickness of the anode oxide film of the aluminum alloy shell prepared by the comparative example is 12 microns, the density is 0.52, and the hardness of the oxide film is 92 HB. alpha-Al in anodic oxide films2O3The content is more than 60 percent.
Effect example 1
(1) Drop test
Assembling a mobile phone by adopting an aluminum alloy shell after anodic oxidation and hole sealing treatment, and respectively observing the cracking condition of an anodic oxide film and the deformation condition of the shell of a sample from a free falling position at a height of 1.5m away from the ground, wherein the cracking schematic diagram of the anodic oxide film is shown in figure 2, and a diagram c is a global diagram of the cracking of the anodic oxide film; the figure a and the figure b are partial enlarged views; wherein the image a is taken perpendicular to the plane of the oxide film and the image b is taken at 45 DEG to the plane of the oxide film.
(2) Adhesion test of anodic oxide film
The adhesion of the anodic oxide film is determined by the Baige test method, in reference to the standard GBT9286-1998 scratch test for paint films of paints and varnishes.
Scribing 10 multiplied by 10 (100) 1 multiplied by 1mm small grids on the surface of the test sample by a hundred grid knife, wherein each scribing line is deep to the bottom layer of the anode film; brushing fragments in the test area with a brush; firmly sticking the tested small grids by using 3M600 size gummed paper or gummed paper with equivalent effect, and wiping the adhesive tape by using an eraser; the same test was performed by grasping one end of the tape by hand and quickly tearing the tape in the vertical direction (90 °) at the same position 2. The peeling area (%) of the anodic film was measured.
(3) Antenna performance testing
And assembling the mobile phone by adopting the aluminum alloy shell subjected to anodic oxidation and hole sealing treatment, and testing the antenna performance of the mobile phone.
The performance tests are shown in the following table:
the experimental results show that:
firstly, when a mobile phone containing the aluminum alloy shell with the anodic oxide film prepared by the invention falls at the height of 1.5m, the surface of the anodic oxide film is not cracked, and the shell is not deformed; and the cracking rate of the aluminum alloy case including the anodic oxide film prepared in the comparative example was as high as 83.3%.
The adhesion of the anodic oxide film is obviously higher than that of the anodic oxide film in a comparative example (prepared by a conventional method), and the adhesion is stable.
The obtained mobile phone has good antenna performance and can continuously and normally work.
Claims (9)
1. A preparation method of an aluminum alloy shell anodic oxide film is characterized by comprising the following steps of carrying out anodic oxidation and hole sealing treatment on an aluminum alloy shell;
the thickness of the side wall of the aluminum alloy shell is more than or equal to 0.85mm, and the smooth transition of the aluminum alloy shell in the thickness direction is more than or equal to 1: 20;
the anodic oxidation conditions are as follows: the oxidation voltage is 11.5V-15V, and the current density is 1.2-2A/dm2The electrolyte is a mixed solution of concentrated sulfuric acid and tartaric acid, the concentration of the electrolyte is 180-200 g/L, and the concentration of the electrolyte refers to the mass-volume ratio of all solutes to a solvent in the electrolyte; the temperature of the electrolyte in the anodic oxidation is 18-21 ℃;
the conditions of the hole sealing treatment are as follows: the concentration of the hole sealing liquid is 12-15 g/L; the temperature of the hole sealing treatment is 80-85 ℃;
the thickness of the anodic oxide film is more than 15 μm.
2. The method of claim 1, wherein the electrolyte concentration is 200 g/L;
and/or the oxidation voltage is 11.5V-12.5V;
and/or the current density is 1.2-1.5A/dm2；
And/or the concentration of the hole sealing liquid is 13-14 g/L.
3. The method of claim 1, wherein the anodizing time is 30 min;
and/or the time of the hole sealing treatment is 15-20 min.
4. The method according to claim 1, wherein the thickness of the anodic oxide film is 15 to 18 μm.
5. The method of claim 1, wherein said anodizing is carried out in an electrolytic cell in which deionized water is replaced at a frequency of 24 hours or less.
6. The preparation method according to any one of claims 1 to 5, wherein before the anodic oxidation, the aluminum alloy shell is washed with deionized water having a conductivity of 35us/cm or less;
and/or the aluminum alloy shell is washed by deionized water after anodic oxidation.
7. An anodized film produced by the production method according to any one of claims 1 to 6, wherein the anodized film has a density of 0.6 or more and a hardness of 100HB or more.
8. An aluminum alloy case comprising the anodic oxide film according to claim 7.
9. A mobile phone comprising the aluminum alloy case of claim 8.
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