CN110524316B - Surface oxidation-based SiCp/Al composite material grinding method - Google Patents
Surface oxidation-based SiCp/Al composite material grinding method Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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- 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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- 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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
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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
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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- 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
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
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Abstract
The invention discloses a method for grinding a SiCp/Al composite material based on surface oxidation, and belongs to the field of material machining. The improvement of the grinding surface quality of the SiCp/Al composite material is realized. Specifically, firstly, the SiCp/Al composite material is subjected to surface oxidation treatment, mainly anodic oxidation treatment and micro-arc oxidation treatment, and Al is formed on the surface layer2O3Oxidizing the ceramic film and then grinding. The invention establishes the grinding condition of coupling removal of SiC particle reinforced phase and Al alloy matrix identity on the grinding surface layer of the SiCp/Al composite material, thereby realizing the novel method and the process for precisely grinding the SiCp/Al composite material. The surface roughness is less than 0.2 μm, so that the quality of the ground surface is greatly improved.
Description
The technical field is as follows:
the invention belongs to the technical field of material machining, and particularly relates to a method for grinding a SiCp/Al composite material based on surface oxidation.
Background art:
the SiCp/Al composite material has the outstanding advantages of high specific strength, specific stiffness, high specific modulus, low thermal expansion coefficient, good thermal conductivity, wear resistance and the like, also has the designability which is incomparable with the traditional alloy material, and as the preparation technology thereof is mature and the performance is improved, the functional elements of the SiCp/Al composite material are increasingly widely applied in the high and new technical fields of aviation, aerospace, electronics and the like. The demand for precise and ultra-precise processing technology of SiCp/Al composite materials is becoming stronger, especially for some parts with higher requirements for surface precision and roughness, such as light high-performance optical devices, precise instruments, electronic packaging, piston reinforcing rings of high-grade automobile engines and the like. For example, in the application of the SiCp/Al composite material in optical and optoelectronic systems, grinding is used as a key process before coating and polishing, and has important influence on subsequent coating and polishing.
Because of the distinct physical and mechanical properties of the SiC particle reinforcement phase and the Al alloy matrix phase, conventional grinding methods have many problems when grinding SiCp/Al composites, such as: 1) due to the hardness difference between SiC particles and an Al alloy matrix, the grinding removal rate has great difference, and the excessive grinding of the Al alloy matrix causes the SiC particles to protrude out of the surface too much. 2) The SiC particles are liable to form through cracks or to be broken under the action of grinding pressure and abrasive grains, resulting in grinding defects. 3) The abrasive and the fallen and broken SiC particles are easily embedded into the surface layer of the Al alloy matrix with lower hardness to form an embedded defect. 4) It is difficult to select the grinding abrasive, the abrasive grain size and the grinding process parameters reasonably. The above problems not only cause damage to the quality of the processed surface, but also directly affect subsequent processing and work, such as coating quality, polishing yield, workpiece performance, and long-term working reliability.
The invention content is as follows:
the present invention is directed to overcoming the above-mentioned disadvantages of the prior art and to provide a SiCp/Al composite material based on surface oxidation and a polishing method, in which Al is formed on the surface layer by oxidizing the surface of the SiCp/Al composite material2O3And oxidizing the ceramic membrane, thereby establishing a grinding condition for coupling and removing the SiC particle reinforced phase and the Al alloy matrix in the same polarity on the grinding surface layer of the SiCp/Al composite material, and realizing the novel method and the process for precisely grinding the SiCp/Al composite material. Specifically, the SiCp/Al composite material is pretreated, then surface oxidation treatment is carried out to obtain an oxide ceramic membrane, and the oxide ceramic membrane is washed with water and dried and then ground to obtain a ground surface with excellent quality. The surface oxidation method mainly comprises anodic oxidation and micro-arc oxidation treatment.
In order to achieve the purpose, the invention adopts the following technical scheme:
a grinding method of SiCp/Al composite material based on surface oxidation comprises the following steps:
(1) taking a SiCp/Al composite material, pretreating the composite material, and oxidizing to obtain an oxide ceramic membrane, so as to finish surface oxidation of the SiCp/Al composite material, wherein the oxidation mode is anodic oxidation or micro-arc oxidation, the thickness of the oxide ceramic membrane is 10-200 mu m, and the surface hardness is 700HV-3000 HV;
(2) and grinding the surface oxidized ceramic film of the SiCp/Al composite material with the oxidized surface by adopting diamond grinding materials with different particle sizes to finish grinding.
In the step (1), when anodic oxidation is adopted, the pretreatment process is as follows: mechanical polishing, alkali washing, water washing, acid washing and water washing; when micro-arc oxidation is adopted, the pretreatment process is as follows: polishing, ultrasonic cleaning and water washing.
In the step (1), when anodic oxidation is adopted, the thickness of the obtained oxide ceramic film is 10-50 μm, and the surface hardness is 700HV-1000 HV; when micro-arc oxidation is adopted, the thickness of the obtained oxide ceramic film is 10-200 mu m, and the surface hardness is 1000HV-3000 HV.
In the step (1), the anodic oxidation treatment process is as follows: the anodic oxidation solution adopted comprises 150-300g/L H2SO41-2g/L oxalic acid and 3-5ml/L glycerol; the oxidation temperature is 10-25 ℃, the oxidation voltage is 12-20V, and the oxidation time is 30-120 min.
In the step (1), the micro-arc oxidation treatment process comprises the following steps: the adopted micro-arc oxidation solution comprises 5g/L to 15g/L of sodium silicate, 1g/L to 3g/L of KOH and Na2WO41g/L-5g/L, 0.5g/L-2.5g/L of nano SiC particles, 20-40 ℃ of oxidation temperature, a bidirectional power supply mode, a positive voltage of 400V-550V, a negative voltage of 50V-100V, a duty ratio of 15% -60%, and an oxidation time of 30min-180 min.
In the step (1), the SiCp/Al composite material surface oxide ceramic membrane obtained by anodic oxidation treatment consists of a porous outer layer and a compact inner layer, and the SiCp/Al composite material surface oxide membrane obtained by anodic oxidation treatment is characterized by Al2O3Wrapping SiC with Al as main component2O3And SiC; the ceramic oxide membrane obtained by micro-arc oxidation treatment is characterized in that the thickness of the membrane layer is larger, the membrane layer grows to the outside and the inside of the matrix, the membrane layer consists of a porous outer layer and a compact inner layer, and the outer layer is mainly Al2O3Mullite, amorphous SiO2And electrolyte-introduced nano SiC, the inner layer mainly comprises mullite and Al2O3And a small amount of matrix SiC particles and nano SiC introduced by electrolyte.
In the step (2), the diamond abrasive granularity is W7-W20.
In the step (2), the quality of the ground SiCp/Al composite material surface is effectively improved, the surface defects are reduced, and a surface with high processing precision and low roughness is obtained, wherein the surface roughness reaches 0.08-0.2 mu m.
In the step (2), the product is positivePreparation of Al by polar oxidation2O3When the ceramic membrane is oxidized: the surface oxide film of the SiCp/Al composite material is characterized by Al2O3Wrapping SiC.
When preparing Al by micro-arc oxidation2O3When the ceramic membrane is oxidized: the surface oxide film of the SiCp/Al composite material is characterized in that a film layer with larger thickness can be prepared by micro-arc oxidation, the film layer grows to the outside and the inside of a matrix, the film layer consists of a porous outer layer and a compact inner layer, the SiC of the outer layer of the film layer is little, and the outer layer is mainly Al2O3And mullite, wherein a small amount of SiC is mainly distributed in the inner layer close to the interface, so that the film structure sequentially contains mullite and Al from the surface to the direction of the matrix2O3A porous outer layer containing mullite and Al2O3And a dense layer of SiC. The outer layer has lower hardness and the inner layer has higher hardness.
The invention has the beneficial effects that:
the invention adopts a surface anodic oxidation or micro-arc oxidation treatment method to carry out pretreatment on the surface to be ground of the SiCp/Al composite material, and Al is formed on the surface of the SiCp/Al composite material2O3And oxidizing the ceramic film. Al in grinding process2O3The oxide ceramic film can have enough holding strength for SiC particles, so that the SiC particles do not slide and roll in the grinding process, and the grinding defects caused by the sliding and rolling are avoided. In addition, during polishing, the abrasive grains first confront the Al on the surface of the Al alloy substrate2O3The ceramic oxide film and the SiC particles are ground, the hardness difference between the ceramic oxide film and the SiC particles is small relative to Al and SiC, the grinding characteristics of the SiC particles and the matrix phase are converged, the condition of realizing isotropic coupling grinding removal of the SiC particles and the matrix is achieved, and the quality of the ground surface is improved.
Description of the drawings:
FIG. 1 is a schematic view of a conventional SiCp/Al composite polishing surface in the prior art, FIG. 1(a) is a schematic view of the surface, FIG. 1(b) is a schematic view of a thickness cross section, in which 1-polishing groove marks are caused by abrasive grains; 2-SiC particles fall off to cause a large number of deep groove marks; 3-raised SiC particles; 4-intact SiC particles; 5-pulling out SiC particles; 6-SiC particles are pressed in;
FIG. 2 is a schematic view showing the polished surface of a surface-oxidized SiCp/Al composite material of example 2 of the present invention, FIG. 2(a) is a schematic view showing the surface, and FIG. 2(b) is a schematic view showing a cross-sectional thickness in which 7-grains cause polishing scratches; 8-intact SiC particles;
FIG. 3 is a SEM image of a polished surface of a conventional SiCp/Al composite material in the prior art;
FIG. 4 is a SEM image of the polished surface of the surface oxidized SiCp/Al composite of example 2 of the present invention.
The specific implementation mode is as follows:
the present invention will be described in further detail with reference to examples.
The SiCp/Al composite materials used in the following examples and comparative examples were SiCp/6061Al composite materials, and the SiC particles had a volume fraction of 56% and a particle diameter of 40 μm and were used as starting materials for producing optical devices after grinding.
Grinding is an important processing procedure of optical devices, and the surface grinding quality has important influence on subsequent nickel plating films and polishing.
Example 1
(1) And carrying out a conventional anodic oxidation pretreatment process on the SiCp/Al composite material sample. Mechanical polishing, alkali washing, water washing, acid washing and water washing to obtain a clean surface. The alkaline washing is carried out by using a 7% NaOH solution with the temperature of 50 ℃ and using a 50% nitric acid solution at room temperature.
Taking a pre-treated SiCp/Al composite material sample as an anode and a lead plate as a cathode, and carrying out anodic oxidation in an anodic oxidation solution to obtain a material with Al on the surface2O3The thickness of the SiCp/Al composite material of the oxide ceramic membrane is 10 mu m, wherein the thickness of the compact inner layer is 3 mu m, the thickness of the porous outer layer is 7 mu m, and the surface hardness is 1000 HV. Wherein, the anodic oxidation aqueous solution comprises the following components: 200g/L of sulfuric acid, 1.5g/L of oxalic acid and 3ml/L of glycerol, and the process parameters are as follows: the voltage is 15V, the temperature is 20 ℃, and the treatment time is 60 min.
And washing and drying the SiCp/Al composite material sample with the anodized surface, and then grinding, wherein the grinding abrasive sequentially selects diamond abrasives with the granularity of W20 and W10, the concentration of the abrasive solution is 8 wt%, the grinding pressure is respectively 2MPa and 1MPa, and the rotating speed is respectively 50r/min and 30 r/min. Grinding for 2min by using a W20 diamond grinding material, removing the porous outer layer, and grinding for 1min by using a W10 diamond grinding material to obtain a ground surface with the roughness of 0.15 mu m, smooth surface and no crack.
Example 2
And carrying out conventional micro-arc oxidation pretreatment process on the SiCp/Al composite material sample. The method comprises the steps of polishing, ultrasonic cleaning and water washing by adopting a conventional micro-arc oxidation pretreatment process. The sanding and polishing adopts 200#, 400#, 600#, 800#, 1000# sand paper, and adopts acetone for ultrasonic cleaning and deionized water for water cleaning.
Taking a pre-treated SiCp/Al composite material sample as an anode and stainless steel as a cathode, and carrying out micro-arc oxidation treatment on a micro-arc oxidation solution to obtain a sample with Al on the surface2O3The thickness of the SiCp/Al composite material of the oxide ceramic membrane is 40 mu m, wherein the thickness of the dense layer is 10 mu m, the thickness of the loose layer is 30 mu m, and the surface hardness is 2800 HV. The micro-arc oxidation aqueous solution comprises 10g/L of Na2SiO3，2g/L KOH，Na2WO42g/L, 1.5g/L of nano SiC particles, 25 +/-5 ℃, a bidirectional constant voltage mode, a positive voltage of 450V, a negative voltage of 80V, a duty ratio of 30 percent and an oxidation time of 60 min.
And washing and drying the SiCp/Al composite material sample subjected to surface micro-arc oxidation, and then grinding. The grinding abrasive sequentially selects W20 diamond abrasive and W7 diamond abrasive, the abrasive concentration is 8 wt%, the grinding pressure is 3MPa and 1MPa respectively, and the rotating speed is 50r/min and 30r/min respectively. Grinding for 3min by using a W20 silicon carbide grinding material, removing a loose outer layer, and grinding for 1min by using a W7 diamond grinding material to obtain a ground surface with the roughness of 0.2 mu m, a smooth surface and no cracks.
The SiCp/Al composite material oxidized in the above examples 1-2 is polished to obtain a polished surface of the SiCp/Al composite material as shown in FIG. 2, FIG. 2(a) is a schematic surface view, FIG. 2(b) is a schematic thickness cross-sectional view showing polishing grooves 7 caused by abrasive grains and complete SiC grains 8; an SEM image of the polished surface is shown in FIG. 4. The grinding surface has smooth quality, greatly reduces grinding defects, and can be used as a raw material for preparing optical devices, the roughness and the precision can meet the requirements of subsequent nickel plating films and polishing, the binding force of the nickel plating film is improved by 10 percent compared with that of an unoxidized SiCp/Al composite material, and the polishing yield is improved by 5 percent.
Comparative example:
the method comprises the following steps of directly grinding an unoxidized SiCp/Al composite material by adopting the conventional technology, specifically grinding for 3min by adopting a W20 silicon carbide grinding material, and then grinding for 1min by adopting a W7 diamond grinding material, observing the pulling-out, cutting-off, pressing-in, crushing and a large number of deep grinding marks of SiC particles on the grinding surface, wherein the schematic diagram of the grinding surface of the SiCp/Al composite material is shown in figure 1, figure 1(a) is a schematic surface diagram, figure 1(b) is a schematic thickness section diagram, and the grinding groove marks 1 caused by abrasive particles can be seen in the schematic diagram; a large number of deep furrows 2 caused by the shedding of SiC particles; raised SiC particles 3; complete SiC particles 4; pulling out 5 SiC particles; pressing SiC particles into the mixture 6; an SEM image of the polished surface of the SiCp/Al composite is shown in FIG. 3. In the invention, as shown in the embodiment 1-2, the surface of the SiCp/Al composite material with oxidized surface has only a few shallow grinding marks and micropores, so that the quality of the ground surface is obviously improved compared with the prior art.
Example 3
And carrying out a conventional anodic oxidation pretreatment process on the SiCp/Al composite material sample. Mechanical polishing, alkali washing, water washing, acid washing and water washing to obtain a clean surface. The alkaline washing is carried out by using a 7% NaOH solution with the temperature of 50 ℃ and using a 50% nitric acid solution at room temperature.
Taking a pre-treated SiCp/Al composite material sample as an anode and a lead plate as a cathode, and carrying out anodic oxidation in an anodic oxidation solution to obtain a material with Al on the surface2O3The thickness of the SiCp/Al composite material of the oxide ceramic membrane is 50 mu m, wherein the thickness of the compact inner layer is 10 mu m, the thickness of the porous outer layer is 40 mu m, and the surface hardness is 700 HV. Wherein, the anodic oxidation aqueous solution comprises the following components: 300g/L of sulfuric acid, 2g/L of oxalic acid and 5ml/L of glycerol, and the process parameters are as follows: the voltage is 20V, the temperature is 20 ℃, and the treatment time is 120 min.
And washing and drying the SiCp/Al composite material sample with the anodized surface, and then grinding. The grinding abrasive sequentially selects diamond abrasive with the granularity of W20 and W10, the concentration of the abrasive solution is 8 wt%, the grinding pressure is 2MPa and 1MPa respectively, and the rotating speed is 50r/min and 30r/min respectively. Grinding for 5min by using a W20 diamond grinding material, removing the porous outer layer, and grinding for 5min by using a W10 diamond grinding material to obtain a ground surface with the roughness of 0.1 mu m, smooth surface and no crack.
Example 4
And carrying out conventional micro-arc oxidation pretreatment process on the SiCp/Al composite material sample. The method comprises the steps of polishing, ultrasonic cleaning and water washing by adopting a conventional micro-arc oxidation pretreatment process. The sanding and polishing adopts 200#, 400#, 600#, 800#, 1000# sand paper, and adopts acetone for ultrasonic cleaning and deionized water for water cleaning.
Taking a pre-treated SiCp/Al composite material sample as an anode and stainless steel as a cathode, and carrying out micro-arc oxidation treatment on a micro-arc oxidation solution to obtain a sample with Al on the surface2O3The thickness of the SiCp/Al composite material of the oxide ceramic membrane is 200 mu m, wherein the thickness of the dense layer is 100 mu m, the thickness of the loose layer is 100 mu m, and the surface hardness is 1000 HV. The micro-arc oxidation aqueous solution contains 15g/L of Na2SiO3，3g/L KOH，Na2WO45g/L, 2.5g/L of nano SiC particles, 25 +/-5 ℃, a bidirectional constant voltage mode, a positive voltage of 550V, a negative voltage of 100V, a duty ratio of 45 percent and an oxidation time of 180 min.
And washing and drying the SiCp/Al composite material sample subjected to surface micro-arc oxidation, and then grinding. The grinding abrasive sequentially selects W20 diamond abrasive and W7 diamond abrasive, the abrasive concentration is 8 wt%, the grinding pressure is 3MPa and 1MPa respectively, and the rotating speed is 50r/min and 30r/min respectively. Grinding for 8min by using a W20 silicon carbide grinding material, removing a loose outer layer, and grinding for 10min by using a W7 diamond grinding material to obtain a ground surface with the roughness of 0.1 mu m, a smooth surface and no cracks.
The grinding surface has smooth quality, greatly reduces grinding defects, and can be used as a raw material for preparing optical devices, the roughness and the precision can meet the requirements of subsequent nickel plating films and polishing, the binding force of the nickel plating film is improved by 15 percent compared with that of an unoxidized SiCp/Al composite material, and the polishing yield is improved by 8 percent.
Claims (4)
1. A method for grinding SiCp/Al composite material based on surface oxidation is characterized by comprising the following steps:
(1) taking SiCp/Al complexCombining materials, carrying out pretreatment on the composite material, then carrying out oxidation to obtain an oxidation ceramic membrane, and finishing the surface oxidation of the SiCp/Al composite material, wherein the oxidation mode is anodic oxidation or micro-arc oxidation, the thickness of the oxidation ceramic membrane is 10-200 mu m, the surface hardness is 700-3000HV, and the anodic oxidation treatment process is as follows: the anodic oxidation solution adopted comprises 150-300g/L H2SO41-2g/L oxalic acid and 3-5ml/L glycerol; the oxidation temperature is 10-25 ℃, the oxidation voltage is 12-20V, and the oxidation time is 30-120 min; the micro-arc oxidation treatment process comprises the following steps: the adopted micro-arc oxidation solution comprises 5-15g/L of sodium silicate, 1-3g/L of KOH and Na2WO4 1-5g/L, 0.5-2.5g/L of nano SiC particles, 20-40 ℃ of oxidation temperature, a bidirectional power supply mode, 400-550V of positive voltage, 50-100V of negative voltage, 15-60% of duty ratio and 30-180min of oxidation time;
(2) and grinding the surface oxidized ceramic membrane of the SiCp/Al composite material after surface oxidation by adopting diamond grinding materials with different particle sizes to finish grinding, wherein the ground SiCp/Al composite material has good surface quality and the surface roughness reaches 0.08-0.2 mu m.
2. The method as claimed in claim 1, wherein in step (1), when anodic oxidation is adopted, the thickness of the obtained oxide ceramic film is 10-50 μm, and the surface hardness is 700-1000 HV; when micro-arc oxidation is adopted, the thickness of the obtained oxide ceramic film is 10-200 μm, and the surface hardness is 1000-3000 HV.
3. The method for grinding SiCp/Al composite material based on surface oxidation as claimed in claim 1, wherein in step (1), the SiCp/Al composite material surface oxidation ceramic film obtained by anodic oxidation treatment consists of a porous outer layer and a compact barrier layer, and the oxide film structure is Al2O3Encapsulating SiC with Al as the component2O3And SiC; the oxide ceramic film obtained by micro-arc oxidation treatment grows towards the outside and the inside of the matrix, the film consists of a porous outer layer and a compact inner layer, and the outer layer comprises Al2O3Mullite, amorphous SiO2And electrolyte-introduced nano SiC, the inner layer comprising mullite and Al2O3And matrix SiC particles and nano SiC introduced by electrolyte.
4. The method for grinding a surface oxidation based SiCp/Al composite material as claimed in claim 1, wherein in the step (2), the diamond grit size is W7-W20.
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