CN108823626A - A kind of Al2O3/ Al/Mg stratiform density gradient material and its preparation method and application - Google Patents
A kind of Al2O3/ Al/Mg stratiform density gradient material and its preparation method and application Download PDFInfo
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- CN108823626A CN108823626A CN201810518126.6A CN201810518126A CN108823626A CN 108823626 A CN108823626 A CN 108823626A CN 201810518126 A CN201810518126 A CN 201810518126A CN 108823626 A CN108823626 A CN 108823626A
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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
- C25D11/026—Anodisation with spark discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/017—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of aluminium or an aluminium alloy, another layer being formed of an alloy based on a non ferrous metal other than aluminium
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
Present invention relates particularly to a kind of ultra-thin Al2O3/ Al/Mg stratiform density gradient material and its preparation method and application.The Al2O3/ Al/Mg density gradient material includes Al2O3Layer, Al layers or aluminium alloy layer, Mg layers or Mg alloy-layer;The Al2O3Layer is prepared using differential arc oxidation in aluminum or aluminum alloy surface in situ, the Al2O3Layer with a thickness of 20-100 microns;The Al2O3The thickness ratio of layer and Al layers or aluminium alloy layer is 1-5:10-25;Described Al layers or interface bond strength between aluminium alloy layer and Mg layers or Mg alloy-layer are more than or equal to 25MPa.Preparation method is:The thicker Al of compacted zone is obtained in a short time based on differential arc oxidization technique by designing electrolyte2O3/ Al/Mg stratiform density gradient material.Of the invention designed and preparation Al2O3/Al/Mg density gradient material, with high surface hardness, it can be achieved that the kinetic energy of efficient absorption and dissipation fragment.It is especially suitable for aerospace fields.
Description
Technical field
The present invention relates to a kind of functionally gradient material (FGM) and its technology of preparing based on aerospace applications, and in particular to a kind of ultra-thin
Al2O3/ Al/Mg stratiform density gradient material and its preparation method and application.
Background technique
Magnesium alloy and aluminium alloy are widely used in aviation boat due to its high elastic modulus, low-density and other excellent properties
It, the fields such as defence and military.Mg/Al lightweight functionally gradient material (FGM) combines the excellent properties of magnesium alloy and aluminium alloy, Ke Yiji
The requirement of performance needed for the earth meets lightweight and structural member.Field especially is protected in the hypervelocity impact of space, Mg/Al is light
Matter functionally gradient material (FGM) is a kind of novel spacecraft barrier material, has good protection when by space junk hypervelocity impact
Performance, this is because the density of Mg/Al lightweight functionally gradient material (FGM), ingredient composition and performance be from side to other side change of gradient,
The propagation law that shock wave can be changed during hypervelocity impact converts interior energy for more space junk kinetic energy, realizes
Protection to in-orbit spacecraft.But simple Mg/Al lightweight functionally gradient material (FGM) its to the breaking capacity for just entering fragment, there are also to be strengthened.
Meanwhile associated analog experiment shows that density gradient material surface hardness is higher, and it is stronger to the breaking capacity for just entering fragment, it realizes
Efficient absorption and dissipation fragment kinetic energy achieve the purpose that reduction and disperse incident space junk kinetic energy, can effectively realize to space flight
The protection of device.Al2O3Belong to ceramic material, with the hardness that metal material hardly matches, in fine and close situation, density 3.8g/
Cm3 is bigger than aluminium alloy and magnesium alloy density.There is differential arc oxidation in aluminium and aluminum alloy surface in-situ preparation alumina ceramic layer at present
Process for treating surface;But weaker zone presence is inevitably had in alumina layer obtained by existing Microarc Oxidation Surface Treatment technology.And
And weaker zone thickness be generally 10-20 microns it is even thicker;Surface porosity layer is due to short texture, low density, and gap is big etc.
Feature, causes its hardness lower, and removal is generally required in practical process.Removal weaker zone not only increases the complexity of technique
Property, while the integral thickness of micro-arc oxidation ceramic layer is also reduced, the microstructure of compacted zone is destroyed, differential arc oxidization technique is hindered
Application in practical projects.
Summary of the invention
It is an object of the invention to be directed to protection of space debris field to novel high surface hardness, lightweight density gradient material
Demand, a kind of high surface hardness Al based on aerospace applications is provided2O3/ Al/Mg stratiform density gradient material and its preparation
Method.
A kind of Al of the present invention2O3/ Al/Mg density gradient material;It includes Al2O3Layer, Al layers or aluminium alloy layer, Mg layers or
Mg alloy-layer;The Al2O3Layer is prepared using differential arc oxidation in aluminum or aluminum alloy surface in situ, the Al2O3The thickness of layer
It is 20-100 microns;The Al2O3The thickness ratio of layer and Al layers or aluminium alloy layer is 1-5:10-25;
Described Al layers or interface bond strength between aluminium alloy layer and Mg layers or Mg alloy-layer are more than or equal to 50MPa.
A kind of Al of the present invention2O3/ Al/Mg density gradient material;Al2O3Layer is made of compacted zone and surface porosity layer;Wherein
The thickness of surface porosity layer is less than 5 μm.
A kind of Al of the present invention2O3/ Al/Mg density gradient material;The material of aluminium alloy layer is selected from Al-Mg alloy, Al-Mn
It is alloy, Al-Cu-Mg alloy, Al-Mg-Si system alloy, Al-Cu-Mg-Fe-Ni system alloy, Al-Zn-Mg-Cu system alloy
One of.
A kind of Al of the present invention2O3/ Al/Mg density gradient material;The material of magnesium alloy layer is selected from closes selected from Mg-Al-Zn system
One of gold, Mg-Al-Mn system alloy, Mg-Al-Si system alloy, Mg-Al-Re system alloy.
A kind of Al of the present invention2O3/ Al/Mg density gradient material;The Al2O3/ Al/Mg density gradient material, along gradient material
Expect thickness direction, density changes in layered gradient.
A kind of Al of the present invention2O3/ Al/Mg density gradient material;The Al2O3In/Al/Mg density gradient material, density is most
The maximum density values in big region are 3.8g/cm3。
A kind of Al of the present invention2O3/ Al/Mg density gradient material;The Al2O3In/Al/Mg density gradient material, density is most
The minimum density values of zonule are 1.78g/cm3。
A kind of Al of the present invention2O3The preparation method of/Al/Mg density gradient material, includes the following steps:
Step 1
Using fine aluminium or aluminium alloy plate and magnesium or magnesium alloy plate as raw material, carry out being polishing to surface smoothness being 0.1-3
μm, preferably 0.1-1 μm;Obtain aluminum substrate and magnesium matrix;
Step 2
After surface preparation aluminum substrate obtained by step 1 and magnesium matrix lamination, it is fitted into graphite jig, using Vacuum Heat
Pressure furnace is sintered;Under vacuum atmosphere, it is warming up to first using the heating rate that 5-15 DEG C/min is preferably 5-10 DEG C/min
280-320 DEG C, preferably 290-310 DEG C, further preferably 300 DEG C of heat preservation 10-40min be preferably 30 DEG C, after with 5-15
DEG C/heating rate of min is warming up to 460-510 DEG C, 80-150min is kept the temperature, loads 1-10MPa pressure in insulating process;Heat preservation
After with the rate of temperature fall of 5-15 DEG C/min cool the temperature to 280-320 DEG C, keep the temperature 0.5h, with being furnace-cooled to room temperature after heat preservation,
Obtain aluminium/magnesium laminar gradient structure.
Step 3
The resulting aluminium of step 2/magnesium stratified material aluminium surface is carried out being polishing to surface smoothness being 1-10 μm, preferably
1-5μm。
Step 4
Aluminium/magnesium stratified material is packed into surface by micro-arc oxidation device, carries out single side differential arc oxidation;The single side differential arc oxidation
Process is:The device for installing sample is placed in electrolytic cell, is completely disposed at specimen surface in electrolyte and and electrolysis liquid surface
Keeping parallelism, anode line connect differential arc oxidation anode, power on;Differential arc oxidation is carried out, is cleaned and dried after differential arc oxidation
To finished product;
Electrolyte used in differential arc oxidation it include water-soluble silicate, water-soluble tetraborate, rare earth oxide;It is described micro-
In arc oxidation electrolyte, the concentration of hydroxide ion is more than or equal to 0.0125mol/L, preferably 0.0125-0.05mol/L, more
Further preferably 0.025mol/L.
In the micro-arc oxidation electrolyte, the concentration of water-soluble silicate is 5-15g/L, is preferably 8-12g/L, further
Preferably 10g/L.
In the micro-arc oxidation electrolyte, the concentration of water-soluble tetraborate is 3-10g/L, preferably 4-10g/L, into one
Step is preferably 4g/L, 6g/L, 10g/L.In the present invention, after other components are quantitative and concentration determines, water-soluble tetraboric acid
The concentration of salt cannot be too high or too low;The too low thickness for also leading to weaker zone increases;It is too high that there is also the same problems.Exist simultaneously
In research process, it was found that after other components optimization, water-soluble tetraborate is sodium tetraborate when being 4g/L, obtains in 15min
The product for being 52 microns to compact oxidation layer, and product of the weaker zone less than 5 microns;And the hardness of products obtained therefrom compact oxidation layer
Greater than 1350HV.The bond strength of compact oxidation layer and matrix is 56MPa.
In the micro-arc oxidation electrolyte, the concentration of rare earth oxide is 0.1-1g/L, preferably 0.4-0.6g/L, into one
Step is preferably 0.5g/L.The rare earth oxide is preferably at least one of yttrium oxide, cerium oxide;Further preferably aoxidize
Yttrium.
Water-soluble silicate is selected from least one of sodium metasilicate, potassium silicate in the micro-arc oxidation electrolyte;Preferably
Sodium metasilicate.
Water-soluble tetraborate is selected from least one of sodium tetraborate, dipotassium tetraborate in the micro-arc oxidation electrolyte;
Preferably sodium tetraborate.
Sodium hydroxide and/or potassium hydroxide and/or ammonium hydroxide is added by the differential arc oxidation electricity in the micro-arc oxidation electrolyte
It solves in liquid, the concentration of hydroxide ion is controlled in 0.0125-0.05mol/L.
The granularity of the micro-arc oxidation electrolyte middle rare earth is 20-40nm.
Above-mentioned sodium metasilicate, sodium tetraborate, sodium hydroxide are that analytical chemistry is pure.Yttrium oxide is 20-40nm powder.Wherein fit
The sodium metasilicate of amount is main film-former;Sodium tetraborate provides the stable element of oxidation ceramic layer as additive, guarantees oxidation pottery
The consistency of enamel coating;Sodium hydroxide improves the conductivity of electrolyte as conductive agent;Yttrium oxide as diffusing particle reinforced phase,
Enter ceramic layer in film forming procedure, improves the structure and performance of ceramic layer, so must be strictly controlled the grain of rare earth oxide
Degree.
The technological parameter of differential arc oxidation is:
Constant current mode;
Current density 10-20A/dm2,
Frequency 300-1000Hz,
Duty ratio 10-30%,
Time 5-120min,
The cleaning is ultrasonic cleaning, and the time of cleaning is 5-15min.The temperature of the drying is 30-60 DEG C.
As the selection process of differential arc oxidation, technological parameter is:
Constant current mode;
Current density 15-17A/dm2,
Frequency 450-550Hz,
Duty ratio 13-16%,
Time 5-20min.
A kind of Al of the present invention2O3The preparation method of/Al/Mg density gradient material,;In 5-20min, compacted zone is obtained
Oxidation ceramic layer of the thickness of surface porosity layer less than 5 μm with a thickness of 40-60 μm;And the knot of oxidation ceramic layer and aluminium alloy plate
Intensity is closed to be more than or equal to 45MPa, be preferably greater than to be equal to 50MPa.
A kind of Al of the present invention2O3The preparation method of/Al/Mg density gradient material;In 5-15min, advanced optimize technique
Afterwards even can be in 5-10min, obtaining dense layer thickness is 40-60 μm and oxidation ceramic layer of the surface porosity layer less than 5 μm;
The hardness of the compacted zone is greater than 1350Hv;Reach as high as 1800HV.
The application of of the invention designed and preparation Al2O3/Al/Mg density gradient material;The application includes being used
Make protective materials.The protective materials is protective materials needed for aerospace field.
The present invention is compared to the prior art compared with having the following advantages that:
Al2O3/Al/Mg density gradient material prepared by the present invention is able to satisfy aerospace field to efficient with kinetic energy
The urgent need of the novel light protective materials of dissipation characteristic.
The Al2O3/Al/Mg density gradient material of preparation in 3 present invention has high surface hardness, it can be achieved that efficiently inhaling
Receive the kinetic energy with dissipation fragment.
Al2O3 ceramic layer is prepared in situ using differential arc oxidation in the present invention, high with Al substrate combinating strength.
Al2O3/Al/Mg density gradient material prepared by the present invention, each interlayer ingredient distribution gradient, through-thickness material
Material performance changes in gradient.
Detailed description of the invention
Fig. 1 is the designed section structure figure with the Al2O3/Al/Mg stratiform density gradient material of preparation of embodiment 1;
As seen from Figure 1, it will be apparent that be divided into 3 layers.
Specific embodiment
Embodiment 1
Design Al2O3Each thickness degree of/Al/Mg density gradient material, Al2O3Thickness is 52 microns, Al thickness is 0.5 millimeter,
Mg thickness is 0.8 millimeter.
Sodium metasilicate of the micro-arc oxidation electrolyte of embodiment 1 by 10g/L, the sodium tetraborate of 4g/L, the sodium hydroxide of 1g/L,
0.5g/L yttrium oxide (its granularity is 20-40nm) composition.
It selects with a thickness of aluminum layer thickness+Al in finished product2O3Layer is with a thickness of aluminium sheet;The magnesium plate of 1.5 millimeters thicks is selected,
Step 1
Using aluminium sheet and magnesium plate as raw material, carry out being polishing to surface smoothness being 1 μm;Obtain aluminum substrate and magnesium matrix;
Step 2
After surface preparation aluminum substrate obtained by step 1 and magnesium matrix lamination, it is fitted into graphite jig, using Vacuum Heat
Pressure furnace is sintered.Under vacuum atmosphere, first using 10 DEG C/min heating rate be warming up to 300 DEG C keep the temperature 30 DEG C, after with
The heating rate of 15 DEG C/min is warming up to 510 DEG C, keeps the temperature 150min, loads 10MPa pressure in insulating process;After heat preservation with
The rate of temperature fall of 15 DEG C/min cools the temperature to 320 DEG C, keeps the temperature 0.5h with room temperature is furnace-cooled to after heat preservation and obtains aluminium/magnesium stratiform
Gradient-structure;
Step 3
The resulting aluminium of step 2/magnesium stratified material aluminium surface is carried out being polishing to surface smoothness being 5 μm,;
Step 4
Aluminium/magnesium stratified material is packed into surface by micro-arc oxidation device, carries out single side differential arc oxidation;The single side differential arc oxidation
Process is:The device for installing sample is placed in electrolytic cell, is completely disposed at specimen surface in electrolyte and and electrolysis liquid surface
Keeping parallelism, anode line connect differential arc oxidation anode, power on;Differential arc oxidation is carried out, is cleaned and dried after differential arc oxidation
To finished product;
The application implementation scheme of micro-arc oxidation electrolyte is:Aluminium sheet is placed in micro-arc oxidation electrolyte, differential of the arc oxygen is carried out
Change, is cleaned and dried to obtain finished product after differential arc oxidation;The technological parameter of differential arc oxidation is:Current density 16A/dm2;Frequency
500Hz;Duty ratio 15%;Time 15min.
The cleaning is ultrasonic cleaning, and the time of cleaning is 10min.The temperature of the drying is 60 DEG C of
In embodiment 1, the product that compact oxidation layer is 52 microns has been obtained in a very short period of time, and weaker zone is less than 5
Micron.In 1 products obtained therefrom of embodiment, the hardness of compact oxidation layer is greater than 1350HV.The bond strength of compact oxidation layer and matrix
For 56MPa.
Embodiment 2
Other conditions are consistent with embodiment 1;The difference is that:
Sodium metasilicate of the micro-arc oxidation electrolyte of embodiment 2 by 5g/L, the sodium tetraborate of 3g/L, the hydroxide of 0.5g/L
Sodium, 0.1g/L yttrium oxide composition.
The application implementation scheme of micro-arc oxidation electrolyte is:Aluminium alloy plate is placed in micro-arc oxidation electrolyte, is carried out micro-
Arc aoxidizes, and is cleaned and dried to obtain finished product after differential arc oxidation;The technological parameter of differential arc oxidation is:Current density 16A/dm2;Frequency
500Hz;Duty ratio 15%;Time 15min.
The cleaning is ultrasonic cleaning, and the time of cleaning is 10min.The temperature of the drying is 60 DEG C of
In embodiment 2, the product that compact oxidation layer is 45 microns has been obtained in a very short period of time, and weaker zone is less than 5
Micron.In 1 products obtained therefrom of embodiment, the hardness of compact oxidation layer is greater than 1350HV.The bond strength of compact oxidation layer and matrix
For 52MPa.
Embodiment 3
Other conditions are consistent with embodiment 1;The difference is that:
Sodium metasilicate of the micro-arc oxidation electrolyte of embodiment 3 by 15g/L, the sodium tetraborate of 10g/L, the hydroxide of 2g/L
Sodium, 1g/L yttrium oxide (its granularity is 20-40nm) composition.
The application implementation scheme of micro-arc oxidation electrolyte is:Aluminium alloy plate is placed in micro-arc oxidation electrolyte, is carried out micro-
Arc aoxidizes, and is cleaned and dried to obtain finished product after differential arc oxidation;The technological parameter of differential arc oxidation is:Constant current mode;Current density
16A/dm2;Frequency 500Hz;Duty ratio 15%;Time 10min.
The cleaning is ultrasonic cleaning, and the time of cleaning is 10min.The temperature of the drying is 60 DEG C of
In embodiment 3, the product that compact oxidation layer is 64 microns has been obtained in a very short period of time, and weaker zone is less than 5
Micron.In 1 products obtained therefrom of embodiment, the hardness of compact oxidation layer is greater than 1350HV.The bond strength of compact oxidation layer and matrix
For 46MPa.
Embodiment 4
Other conditions are consistent with embodiment 1;The difference is that:
Sodium metasilicate of the micro-arc oxidation electrolyte of embodiment 4 by 8g/L, the sodium tetraborate of 6g/L, the sodium hydroxide of 1g/L,
0.6g/L yttrium oxide (its granularity is 20-40nm) composition.
The application implementation scheme of micro-arc oxidation electrolyte is:Aluminium alloy plate is placed in micro-arc oxidation electrolyte, is carried out micro-
Arc aoxidizes, and is cleaned and dried to obtain finished product after differential arc oxidation;The technological parameter of differential arc oxidation is:Constant current mode;Current density
16A/dm2;Frequency 500Hz;Duty ratio 15%;Time 5min.
The cleaning is ultrasonic cleaning, and the time of cleaning is 10min.The temperature of the drying is 60 DEG C of
In embodiment 4, the product that compact oxidation layer is 53 microns has been obtained in a very short period of time, and weaker zone is less than 5
Micron.In 1 products obtained therefrom of embodiment, the hardness of compact oxidation layer is greater than 1200HV.The bond strength of compact oxidation layer and matrix
For 50MPa.
Comparative example 1
Other conditions are consistent with embodiment 1;The difference is that:
Sodium metasilicate of the micro-arc oxidation electrolyte of comparative example 1 by 10g/L, the sodium tetraborate of 0g/L, the sodium hydroxide of 1g/L,
0.5g/L yttrium oxide (its granularity is 20-40nm) composition.
In comparative example 1, the product that compact oxidation layer is only 32 microns is obtained, and weaker zone is 12 microns.1 institute of comparative example
It obtains in product, the hardness of compact oxidation layer is only 946HV.The bond strength of compact oxidation layer and matrix is only 37MPa.
Comparative example 2
Other conditions are consistent with embodiment 1;The difference is that:
Sodium metasilicate of the micro-arc oxidation electrolyte of comparative example 2 by 20g/L, the sodium tetraborate of 15g/L, the hydroxide of 0g/L
Sodium, 1.5g/L yttrium oxide (its granularity is 20-40nm) composition.
In comparative example 2, the product that compact oxidation layer is only 67 microns is obtained, and weaker zone is 17 microns.1 institute of comparative example
It obtains in product, the hardness of compact oxidation layer is only 1016HV.The bond strength of compact oxidation layer and matrix is only 46MPa.
Comparative example 3
Other conditions are consistent with embodiment 1;The difference is that:
Sodium metasilicate of the micro-arc oxidation electrolyte of comparative example 3 by 2g/L, the sodium tetraborate of 15g/L, the sodium hydroxide of 3g/L,
1.5g/L yttrium oxide (its granularity is 20-40nm) composition.
In comparative example 3, the product that compact oxidation layer is only 47 microns is obtained, and weaker zone is 15 microns.1 institute of comparative example
It obtains in product, the hardness of compact oxidation layer is only 1042HV.The bond strength of compact oxidation layer and matrix is only 43MPa.Simultaneously
The cost of the comparative example is much higher than the embodiment of the present invention.
Claims (10)
1. a kind of Al2O3/ Al/Mg density gradient material;It is characterized in that:The Al2O3/ Al/Mg density gradient material includes
Al2O3Layer, Al layers or aluminium alloy layer, Mg layers or Mg alloy-layer;The Al2O3Layer is using differential arc oxidation on aluminum or aluminum alloy surface
It is prepared in situ, the Al2O3Layer with a thickness of 20-100 microns;The Al2O3Layer and Al layers or the thickness ratio of aluminium alloy layer
For 1-5:10-25;
Described Al layers or interface bond strength between aluminium alloy layer and Mg layers or Mg alloy-layer are more than or equal to 25MPa.
2. a kind of Al according to claim 12O3/ Al/Mg density gradient material;It is characterized in that:Al2O3Layer is by compacted zone
It is formed with surface porosity layer;Wherein the thickness of surface porosity layer is less than 10 μm.
3. a kind of Al according to claim 12O3/ Al/Mg density gradient material;It is characterized in that:
The material of aluminium alloy layer be selected from Al-Mg alloy, Al-Mn system alloy, Al-Cu-Mg alloy, Al-Mg-Si system alloy,
One of Al-Cu-Mg-Fe-Ni system alloy, Al-Zn-Mg-Cu system alloy;
The material of magnesium alloy layer is selected from Mg-Al-Zn alloy, Mg-Al-Mn system alloy, Mg-Al-Si system alloy, Mg-Al-
One of Re system alloy.
4. a kind of Al according to claim 12O3/ Al/Mg density gradient material;It is characterized in that:The Al2O3/Al/Mg
Density gradient material, along functionally gradient material (FGM) thickness direction, density changes in layered gradient.
5. a kind of Al according to claim 12O3/ Al/Mg density gradient material;It is characterized in that:The Al2O3/Al/Mg
In density gradient material, the maximum density values of density maximum region are 3.8g/cm3, the minimum density values of density Minimum Area are
1.78g/cm3。
6. a kind of prepare the Al as described in claim 1-5 any one2O3The method of/Al/Mg density gradient material, feature exist
In;Include the following steps:
Step 1
Using fine aluminium or aluminium alloy plate and magnesium or magnesium alloy plate as raw material, carry out being polishing to surface smoothness being 0.1-3 μm, it is excellent
It is selected as 0.1-1 μm.Obtain aluminum substrate and magnesium matrix;
Step 2
After surface preparation aluminum substrate obtained by step 1 and magnesium matrix lamination, it is fitted into graphite jig, using vacuum hotpressing stove
It is sintered.Under vacuum atmosphere, 280- is warming up to using the heating rate that 5-15 DEG C/min is preferably 5-10 DEG C/min first
320 DEG C, preferably 290-310 DEG C, further preferably 300 DEG C of heat preservation 10-40min be preferably 30 DEG C, after with 5-15 DEG C/min
Heating rate be warming up to 460-510 DEG C, keep the temperature 80-150min, load 1-10MPa pressure in insulating process;After heat preservation
Cool the temperature to 280-320 DEG C with the rate of temperature fall of 5-15 DEG C/min, keep the temperature 0.5h, with room temperature is furnace-cooled to after heat preservation, obtain aluminium/
Magnesium laminar gradient structure;
Step 3
The resulting aluminium of step 2/magnesium stratified material aluminium surface is carried out being polishing to surface smoothness being 1-10 μm, preferably 1-5 μ
m。
Step 4
Aluminium/magnesium stratified material is packed into surface by micro-arc oxidation device, carries out single side differential arc oxidation;The single side micro-arc oxidation process
For:The device for installing sample is placed in electrolytic cell, specimen surface is made to be completely disposed in electrolyte and keep with electrolysis liquid surface
In parallel, anode line connects differential arc oxidation anode, powers on;Differential arc oxidation is carried out, is cleaned and dried to obtain into after differential arc oxidation
Product;
Electrolyte used in differential arc oxidation it include water-soluble silicate, water-soluble tetraborate, rare earth oxide;The differential of the arc oxygen
Change in electrolyte, the concentration of hydroxide ion is more than or equal to 0.0125mol/L, preferably 0.0125-0.05mol/L, more into one
Step is preferably 0.025mol/L;
In the micro-arc oxidation electrolyte, the concentration of water-soluble silicate is 5-15g/L, is preferably 8-12g/L, further preferably
For 10g/L;
In the micro-arc oxidation electrolyte, the concentration of water-soluble tetraborate is 3-10g/L, is preferably 3-6g/L, is further excellent
It is selected as 4g/L;
In the micro-arc oxidation electrolyte, the concentration of rare earth oxide is 0.1-1g/L, is preferably 0.4-0.6g/L, is further excellent
It is selected as 0.5g/L.
7. a kind of Al according to claim 62O3The preparation method of/Al/Mg density gradient material, it is characterised in that:
Water-soluble silicate is selected from least one of sodium metasilicate, potassium silicate in the micro-arc oxidation electrolyte;Preferably silicic acid
Sodium.
Water-soluble tetraborate is selected from least one of sodium tetraborate, dipotassium tetraborate in the micro-arc oxidation electrolyte;It is preferred that
For sodium tetraborate.
Sodium hydroxide and/or potassium hydroxide and/or ammonium hydroxide is added by the micro-arc oxidation electrolyte in the micro-arc oxidation electrolyte
In, the concentration of hydroxide ion is controlled in 0.0125-0.05mol/L;
The granularity of the micro-arc oxidation electrolyte middle rare earth is 20-40nm;
The technological parameter of differential arc oxidation is:
Constant current mode;
Current density 10-20A/dm2,
Frequency 300-1000Hz,
Duty ratio 10-30%,
Time 5-120min.
8. a kind of Al according to claim 62O3The preparation method of/Al/Mg density gradient material, it is characterised in that:
In 10-20min, oxide ceramic of the thickness less than 5 μm of surface porosity layer with a thickness of 40-60 μm of compacted zone is obtained
Layer;And the bond strength of oxidation ceramic layer and aluminium alloy plate is more than or equal to 50MPa.
9. a kind of Al according to claim 62O3The preparation method of/Al/Mg density gradient material, it is characterised in that:
In 10-20min, obtaining dense layer thickness is 40-60 μm and oxidation ceramic layer of the surface porosity layer less than 5 μm;It is described
The hardness of compacted zone is greater than 1350Hv;Reach as high as 1800HV.
10. one kind Al as described in claim 1-5 any one2O3The application of/Al/Mg density gradient material;It is characterized in that:
The application includes being used as protective materials;The protective materials is protective materials needed for aerospace field.
Priority Applications (1)
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