CN115044959B - Corrosive for testing diamond/aluminum-silicon composite material interface and using method thereof - Google Patents
Corrosive for testing diamond/aluminum-silicon composite material interface and using method thereof Download PDFInfo
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Abstract
The invention discloses a corrosive for inspecting a diamond/aluminum-silicon composite material interface, which comprises a corrosive solution I and a corrosive solution II, wherein the corrosive solution I comprises nitric acid, glycerol and water; the corrosion solution II comprises hydrofluoric acid, hypophosphorous acid, glycerol and water; the using method of the corrosive comprises the following steps: (1) Processing the sample into a slice sample, polishing, cleaning and drying; (2) electrolytic etching of the sample in an etching solution I; (3) Electrolytic etching the sample of (2) in an etching solution II; (4) Observing the interface between diamond and aluminum matrix and its reaction product under scanning electron microscope; the corrosive agent can clearly and completely display Al at the interface of the diamond/aluminum-silicon composite material 4 C 3 The morphology of the phase and the silicon phase is high in efficiency, good in reproducibility and simple in operation.
Description
Technical Field
The invention relates to a material interface corrosive agent, in particular to a corrosive agent for testing a diamond/aluminum-silicon composite material interface and a use method thereof.
Background
The diamond/aluminum composite material has high heat conductivity, low thermal expansion coefficient and low density, and is particularly suitable for being used as a high-performance electronic packaging heat dissipation material for chip semiconductors such as GaAs and GaN. The preparation method of the diamond/aluminum composite material mainly comprises two main types of powder metallurgy sintering method and melt pressure infiltration method, wherein the composite material prepared by the powder metallurgy sintering method and the melt pressure infiltration method has higher heat conductivity coefficient (the volume fraction of diamond particles can reach 65 percent) and can form special-shaped pieces, thereby having more development prospect. In the case of melt pressure infiltration, when the molten aluminum is immersed in the gaps between diamond particles, al is formed by nucleation and growth due to interdiffusion of elements at the contact point of diamond and molten aluminum 4 C 3 The phase, this interfacial product can increase interfacial binding force and thus effectively increase the thermal conductivity of the material, but on the other hand, due to Al 4 C 3 The phase has low thermal conductivity and hygroscopicity, and excessive Al 4 C 3 The phase not only reduces the thermal conductivity of the composite materialAnd also reduces its long-term service performance. The properties of the composite material are largely dependent on the interface structure, and for this reason, it is necessary to find a material that effectively displays Al at the diamond/aluminum composite interface 4 C 3 The corrosive agent with the morphology and distribution of the phase and the inspection method thereof can effectively control the structure and the performance of the phase by adjusting the preparation process.
Several documents have disclosed corrosive agents for detecting diamond/aluminum composite interfaces and detection methods thereof: S.Kleiner et Al adopts a pneumatic melt infiltration method to prepare diamond/pure aluminum composite material, samples are broken, electrochemical corrosion is carried out in nitric acid aqueous solution to remove aluminum matrix, and then Al on the surface of the diamond can be observed under a scanning electron microscope 4 C 3 Phase formation (S.Kleiner, effect of diamond crystallographic orientation on dissolution and carbide formation in contact with liquid aluminium, scripta Materialia, 55 (2006) 291-294). However, this document does not describe the concentration of the aqueous nitric acid solution and the electrochemical corrosion parameters (such as the current density of the corroded area, the corrosion time, etc.), and the difficulty of control in actual operation is high. E.Monje et al prepared diamond/pure aluminum composite material by air pressure melt infiltration method, designed a special device for electrochemical corrosion of sample: inserting a rod-shaped sample (cathode) into a hollow cylindrical body (anode) made of copper, adopting O-shaped sealing rings at the upper and lower ends of the inner side of the hollow cylindrical body, fixing the radial distance between the sample and the hollow cylindrical body to be 3mm, then placing the device in a 10% (volume ratio) nitric acid aqueous solution, and controlling the corrosion current density to be 2A/cm 2 When the etching time is found to be 2.5min, the Al formed on the surface of the diamond can be better observed under a scanning electron microscope 4 C 3 Morphology of the phases (I.E.Monje, aluminum/diamond composites: apreparative method to characterize reactivity and selectivity at the interface, scripta Materialia 66 (2012) 789-792). However, the electrochemical corrosion device provided by the document is complex, and particularly the cylindrical diamond/aluminum composite material is extremely difficult to process and has great practical application difficulty. In addition, in both the above examples, a single aqueous nitric acid solution was used as the etchant, and the interfacial reactant Al 4 C 3 Meeting each otherAnd the aluminum alloy is partially dissolved in corrosive liquid along with the corrosion of the aluminum matrix, so that the real appearance of the aluminum alloy is difficult to display.
In recent years, diamond/aluminum-silicon composite materials have been studied more widely because aluminum-silicon alloys have low melting points and good fluidity, so that the infiltration temperature is significantly lower than that of pure aluminum, the reaction degree of diamond/aluminum matrix interface can be effectively controlled, and excessive Al is avoided 4 C 3 And (3) generating a phase. In addition, the research shows that the silicon phase can be adhered to part of the surface of the diamond, thereby not only reducing Al 4 C 3 The amount of phase formation can further enhance the interfacial bonding force. Al at the diamond/Al-Si composite interface compared to pure aluminum matrix 4 C 3 The amount of phase formation is relatively small, and for this purpose, a novel corrosive agent and an interface inspection method thereof must be found, and firstly, the generation of Al is avoided 4 C 3 The corrosion damage of the phases is avoided, meanwhile, excessive corrosion to the silicon phases is avoided, and finally, the morphology of the two phases can be effectively displayed, so that a basis is provided for the control of the structure and the performance of the composite material.
Disclosure of Invention
The invention aims to: the invention aims to provide a corrosive for testing a diamond/aluminum-silicon composite material interface, which can completely display Al 4 C 3 The morphology of the phase and the silicon phase provides basis for controlling the structure and the performance of the composite material; it is another object of the present invention to provide a method of using the etchant.
The technical scheme is as follows: the etchant for inspecting the diamond/aluminum-silicon composite material interface comprises an etching solution I and an etching solution II, wherein the etching solution I comprises nitric acid, glycerol and water; the corrosion solution II comprises hydrofluoric acid, hypophosphorous acid, glycerol and water.
In the corrosion solution I, nitric acid can rapidly remove a thicker aluminum coating to enable a diamond/aluminum matrix interface to be primarily exposed, and glycerol can inhibit pitting of an aluminum matrix to enable the corrosion removal process of the aluminum matrix to be more uniform.
In the etching solution II, hydrofluoric acid and hypophosphorous acid react Al 4 C 3 Further etching and removing residual aluminum layer around the phaseMeanwhile, the glycerol can make the corrosion removal process of the aluminum matrix more uniform; in addition, hypophosphorous acid also prevents the oxidation of silicon to SiO during electrolysis 2 The aluminum hypophosphite is dissolved by hydrofluoric acid, so that the true appearance of a silicon phase is shown, and the corrosion product aluminum hypophosphite is dissolved in water, so that the continuous corrosion process can be ensured.
Preferably, each 100mL of the corrosion solution I comprises 10-12 mL of nitric acid, 8-10 mL of glycerol and the balance of water; the mass fraction of the nitric acid is 65-70%.
Configuration of the corrosive solution I: taking a small amount of water in a beaker, slowly adding nitric acid into the beaker, stirring the mixture by using a glass rod to ensure that the nitric acid is uniformly mixed, adding glycerol, uniformly stirring the mixture, adding water, mixing the mixture and fixing the volume to 100mL.
Preferably, each 100mL of solution in the corrosion solution II comprises 5-7 mL of hydrofluoric acid, 7-10 mL of hypophosphorous acid and the balance of water; the mass fraction of the hydrofluoric acid is 35-40%; the mass fraction of the hypophosphorous acid is 85-85%.
Configuration of corrosive solution II: taking a small amount of water in a beaker, respectively measuring hydrofluoric acid and hypophosphorous acid, slowly adding the hydrofluoric acid and the hypophosphorous acid into the beaker, stirring the mixture by using a glass rod to ensure that the hydrofluoric acid and the hypophosphorous acid are uniformly mixed, adding glycerol, uniformly stirring the mixture, adding water, mixing the mixture, and fixing the volume to 100mL.
The application method of the corrosive provided by the invention comprises the following steps:
(1) Processing the diamond/aluminum silicon composite material sample into a sheet sample, polishing, cleaning and drying;
(2) Connecting the corrosion sample with the positive electrode of a direct current power supply, connecting the platinum electrode with the negative electrode, putting the positive electrode and the negative electrode into a corrosion solution I, starting the direct current power supply to start electrolytic corrosion, taking out the sample, cleaning and drying;
(3) Connecting the sample in the step (2) with the positive electrode of a direct current power supply, connecting a platinum electrode with a negative electrode, putting the positive electrode and the negative electrode into an etching solution II, starting the direct current power supply to start electrolytic etching, taking out the sample, and cleaning and drying the sample in alcohol;
(4) The interface of diamond and aluminum substrate and its reaction products were observed under a scanning electron microscope.
Preferably, the diamond/aluminum silicon composite material in the step (1) has a weight percentage of silicon in the matrix of 5-9 wt% and the balance of aluminum.
Preferably, the etching solution I in the step (2) has an etching current density of 2A/cm at 25 DEG C 2 The electrolysis time is 10-14 s.
Wherein the corrosion current density is the current intensity of the direct current power supply divided by the area of the aluminum silicon matrix part of the exposed part of the sample, and the area percentage of the aluminum silicon matrix of the exposed part of the sample is equal to the volume percentage of the aluminum silicon matrix in the diamond/aluminum silicon composite material.
Preferably, the etching solution II in the step (3) has an etching current density of 2A/cm at 25 DEG C 2 The electrolysis time is 16-20 s.
Preferably, the step (1) adopts a laser cutting machine to process the diamond/aluminum silicon composite material sample into a sheet-shaped sample, the cut surface is polished, and then the sample is cleaned and dried; and then covering part of the area of the sample by using insulating glue to expose the electrolytic corrosion surface, so as to prepare the corrosion sample.
Preferably, the electrolytic etching area of the etching specimen immersed in the etching solution in the step (2) is 10mm×3mm, and the other portions immersed in the etching solution are covered with an insulating paste.
The mechanism of the invention is as follows: compared with pure aluminum, the aluminum-silicon alloy has low melting point and good fluidity, and the infiltration temperature is obviously lower than that of pure aluminum, so that the Al at the interface of the diamond/aluminum-silicon composite material 4 C 3 The amount of phase formation is small, and for this purpose, al is first avoided 4 C 3 The corrosion damage of the phases is avoided, meanwhile, excessive corrosion to the silicon phases is avoided, and finally, the morphology of the two phases can be effectively displayed. The etchant for testing the diamond-silicon-aluminum composite material comprises an etching solution I and an etching solution II. In the etching solution I, the thicker aluminum coating layer is removed rapidly by the nitric acid aqueous solution, so that the diamond/aluminum matrix interface is primarily exposed, and the glycerol can inhibit the pitting corrosion of the aluminum matrix, so that the corrosion removal process of the aluminum matrix is more uniformBy controlling electrolytic corrosion time to prevent the reaction of Al 4 C 3 The phases cause corrosion damage. In the etching solution II, hydrofluoric acid and hypophosphorous acid react Al 4 C 3 The residual aluminum layer around the phase is further corroded and removed cleanly, and meanwhile, the glycerol can enable the corrosion and removal process of the aluminum matrix to be more uniform; hydrofluoric acid and hypophosphorous acid are mainly used for etching aluminum matrix, but for Al 4 C 3 The corrosion effect of the phase is very small; in addition, hypophosphorous acid has strong reducibility and can prevent silicon oxide from being formed into SiO during electrolysis 2 The aluminum hypophosphite is dissolved by hydrofluoric acid, so that the true appearance of a silicon phase is shown, and the corrosion product aluminum hypophosphite is dissolved in water, so that the continuous corrosion process can be ensured.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages: (1) The corrosive agent can clearly and completely display Al at the interface of the diamond/aluminum-silicon composite material 4 C 3 The morphology of the phase and the silicon phase is high in efficiency and good in reproducibility; (2) Through the adjustment of the formulas of the corrosive agents I and II and the two-step electrolysis process, the Al at the interface is ensured 4 C 3 Complete phase indication, avoiding corrosion to Al with single aqueous nitric acid for long periods of time 4 C 3 Damage to phase morphology; (3) The use method of the corrosive agent has the advantages of simple operation, high efficiency and good reproducibility.
Drawings
FIG. 1 is a photograph of a diamond/aluminum silicon composite interface in example 1;
FIG. 2 is an EDS spectrum of Si particles at the diamond/aluminum silicon composite interface in example 1;
FIG. 3 is a photograph of a diamond/aluminum silicon composite interface in example 2;
FIG. 4 is a photograph of a diamond/aluminum silicon composite interface in example 3;
fig. 5 is a photograph of the diamond/aluminum silicon composite interface of comparative example 1.
Detailed Description
The technical scheme of the invention is further described below by referring to examples.
Example 1
The etchant for inspecting the diamond/aluminum-silicon composite material interface comprises an etching solution I and an etching solution II, wherein the etching solution I comprises the following components: 11mL of nitric acid with mass fraction of 68%, 8mL of glycerol with purity of 99%, and the balance of deionized water; the etching solution II comprises: 7mL of hydrofluoric acid with the mass fraction of 35%, 10mL of hypophosphorous acid with the mass fraction of 80%, 9mL of glycerol with the purity of 99% and the balance of deionized water.
Preparing a corrosion solution I: taking a small amount of deionized water in a beaker, measuring 11mL of nitric acid, slowly adding the nitric acid in the beaker, stirring the nitric acid with a glass rod to uniformly mix the nitric acid and the nitric acid, adding 8mL of glycerol, uniformly stirring the glycerol, adding deionized water, mixing the glycerol and the glycerol, and fixing the volume to 100mL.
Preparing a corrosion solution II: taking a small amount of deionized water in a beaker, respectively weighing 7mL of hydrofluoric acid and 10mL of hypophosphorous acid, slowly adding into the beaker, stirring with a glass rod to uniformly mix the materials, adding 9mL of glycerol, uniformly stirring, and finally adding deionized water to mix and fix the volume to 100mL.
The application method of the corrosive for testing the diamond/aluminum-silicon composite material interface comprises the following steps:
(1) Preparing an electrolytic corrosion sample:
sample 1 was a diamond/aluminum silicon composite (volume fraction of diamond 65vol%; matrix was Al-9wt% Si alloy) prepared by air infiltration (infiltration temperature 630 ℃, air pressure 1.5MPa, diamond/aluminum liquid contact time 3 min). Cutting the composite material into a sheet shape of 10mm multiplied by 2mm by a laser cutting machine, polishing the cut surface, and then cleaning and drying; then, a part of the area of the test piece was covered with an insulating paste to expose an electrolytic etched surface of 10mm×3mm (in which the area of the metal matrix occupied 35% of the area of the composite material), to obtain an etched test piece.
(2) Connecting the corrosion sample with the positive electrode of a direct current power supply, connecting the platinum electrode plate with the negative electrode, then putting the positive electrode and the negative electrode into a corrosion solution I at 25 ℃ to ensure that the electrolytic corrosion surface of the sample is completely immersed in the corrosion solution, turning on the direct current power supply, and regulating the voltage to ensure that the corrosion current density of the metal matrix at the exposed part of the corrosion sample reaches 2A/cm 2 The electrolysis time was 10s, after which the test was taken outWashing and drying the sample in alcohol;
(3) Connecting the corroded sample in step (2) with the positive electrode of a direct current power supply, connecting a platinum electrode with a negative electrode, then putting the positive electrode and the negative electrode into a corrosion solution II at 25 ℃ to ensure that the electrolytic corrosion surface of the sample is completely immersed in the corrosion solution, turning on the direct current power supply, and regulating the voltage to ensure that the corrosion current density of the metal matrix at the exposed part of the corrosion sample reaches 2A/cm 2 The electrolysis time is 18s, and then the sample is taken out, washed in alcohol and dried;
(4) The interface of diamond and aluminum substrate was observed under a scanning electron microscope, and the result is shown in fig. 1.
As can be seen from FIG. 1, al 4 C 3 The phase is thin and granular and is attached to the surface of diamond to grow, and is selectively unevenly distributed on different surfaces. Related studies show that Al 4 C 3 The phase grows readily on the (1 1 1) crystal plane of diamond, while it grows harder on the (1 0) crystal plane (i.e. monje, aluminum/diamond composites: A preparative method to characterize reactivity and selectivity at the interface, scripta Materialia 66 (2012) 789-792), which is consistent with the results of fig. 1. In fig. 1, it can also be seen that coarse particles, which are silicon particles, adhere to the diamond surface, as evidenced by EDS spectra (fig. 2). Therefore, the corrosive and the inspection method thereof can conveniently and effectively inspect the interface structure of the diamond/aluminum-silicon composite material.
Example 2
The etchant for inspecting the diamond/aluminum-silicon composite material interface comprises an etching solution I and an etching solution II, wherein the etching solution I comprises the following components: 10mL of nitric acid with the mass fraction of 70%, 9mL of glycerol with the purity of 99%, and the balance of deionized water; the etching solution II comprises: 6mL of hydrofluoric acid with the mass fraction of 38%, 9mL of hypophosphorous acid with the mass fraction of 83%, 10mL of glycerol with the purity of 99% and the balance of deionized water.
Preparing a corrosion solution I: taking a small amount of deionized water in a beaker, measuring 10mL of nitric acid, slowly adding the nitric acid into the beaker, stirring the nitric acid with a glass rod to uniformly mix the nitric acid and the beaker, adding 9mL of glycerol, uniformly stirring the glycerol, adding deionized water, mixing the glycerol and the deionized water, and fixing the volume to 100mL.
Preparing a corrosion solution II: taking a small amount of deionized water in a beaker, respectively weighing 6mL of hydrofluoric acid and 9mL of hypophosphorous acid, slowly adding into the beaker, stirring with a glass rod to uniformly mix the materials, adding 10mL of glycerol, uniformly stirring, and finally adding deionized water to mix and fix the volume to 100mL.
The application method of the corrosive for testing the diamond/aluminum-silicon composite material interface comprises the following steps:
(1) Preparing an electrolytic corrosion sample:
sample 2 was a diamond/aluminum silicon composite (volume fraction of diamond 64vol%; matrix was Al-5wt% Si alloy) prepared by air infiltration (infiltration temperature 700 ℃, air pressure 1.5MPa, diamond/aluminum liquid contact time 3 min). Cutting the composite material into a sheet shape of 10mm multiplied by 2mm by a laser cutting machine, polishing the cut surface, and then cleaning and drying; then, a part of the area of the test piece was covered with an insulating paste to expose an electrolytic etched surface of 10mm×3mm (in which the area of the metal matrix occupied 36% of the area of the composite material), to obtain an etched test piece.
(2) Connecting the corrosion sample with the positive electrode of a direct current power supply, connecting the platinum electrode plate with the negative electrode, then putting the positive electrode and the negative electrode into a corrosion solution I at 25 ℃ to ensure that the electrolytic corrosion surface of the sample is completely immersed in the corrosion solution, turning on the direct current power supply, and regulating the voltage to ensure that the corrosion current density of the metal matrix at the exposed part of the corrosion sample reaches 2A/cm 2 The electrolysis time is 14s, and then the sample is taken out, washed in alcohol and dried;
(3) Connecting the corroded sample in step (2) with the positive electrode of a direct current power supply, connecting a platinum electrode with a negative electrode, then putting the positive electrode and the negative electrode into a corrosion solution II at 25 ℃ to ensure that the electrolytic corrosion surface of the sample is completely immersed in the corrosion solution, turning on the direct current power supply, and regulating the voltage to ensure that the corrosion current density of the metal matrix at the exposed part of the corrosion sample reaches 2A/cm 2 The electrolysis time is 20s, and then the sample is taken out, washed in alcohol and dried;
(4) The interface of diamond and aluminum substrate was observed under a scanning electron microscope, and the result is shown in fig. 3.
As can be seen from FIG. 3, al 4 C 3 Adhesion of phase and silicon phase to diamond surface, wherein Al 4 C 3 The phases are selectively unevenly distributed on different surfaces of the diamond. As compared with example 1, the impregnation temperature of this example was higher (700 ℃ C.) and the silicon content was reduced (5 wt% Si), so Al was 4 C 3 The phase size increases and the distribution density of the silicon phase decreases. Therefore, the corrosive and the inspection method thereof can conveniently and effectively inspect the interface structure of the diamond/aluminum-silicon composite material.
Example 3
The etchant for inspecting the diamond/aluminum-silicon composite material interface comprises an etching solution I and an etching solution II, wherein the etching solution I comprises the following components: 12mL of 65% nitric acid, 10mL of 99% glycerol, and the balance of deionized water; the etching solution II comprises: 5mL of hydrofluoric acid with the mass fraction of 40%, 7mL of hypophosphorous acid with the mass fraction of 85%, 8mL of glycerol with the purity of 99% and the balance of deionized water.
Preparing a corrosion solution I: taking a small amount of deionized water in a beaker, slowly adding 12mL of nitric acid into the beaker, stirring with a glass rod to uniformly mix the nitric acid and the beaker, adding 10mL of glycerol, uniformly stirring, adding deionized water, mixing and fixing the volume to 100mL.
Preparing a corrosion solution II: taking a small amount of deionized water in a beaker, respectively weighing 5mL of hydrofluoric acid and 7mL of hypophosphorous acid, slowly adding into the beaker, stirring with a glass rod to uniformly mix the materials, adding 8mL of glycerol, uniformly stirring, and finally adding deionized water to mix and fix the volume to 100mL.
The application method of the corrosive for testing the diamond/aluminum-silicon composite material interface comprises the following steps:
(1) Electrolytic corrosion sample preparation
Sample 3 was a diamond/aluminum silicon composite (63 vol% diamond; al-7wt% Si alloy as matrix) prepared by air infiltration (750 ℃ C., 1.5MPa air pressure, 3min diamond/aluminum liquid contact time). Cutting the composite material into a sheet shape of 10mm multiplied by 2mm by a laser cutting machine, polishing the cut surface, and then cleaning and drying; then, a part of the area of the test piece was covered with an insulating paste to expose an electrolytic etched surface of 10mm×3mm (in which the area of the metal matrix occupied 37% of the area of the composite material), to obtain an etched test piece.
(2) Connecting the corrosion sample with the positive electrode of a direct current power supply, connecting the platinum electrode plate with the negative electrode, then putting the positive electrode and the negative electrode into a corrosion solution I at 25 ℃ to ensure that the electrolytic corrosion surface of the sample is completely immersed in the corrosion solution, turning on the direct current power supply, and regulating the voltage to ensure that the corrosion current density of the metal matrix at the exposed part of the corrosion sample reaches 2A/cm 2 The electrolysis time is 12s, and then the sample is taken out, washed in alcohol and dried;
(3) Connecting the corroded sample in step (2) with the positive electrode of a direct current power supply, connecting a platinum electrode with a negative electrode, then putting the positive electrode and the negative electrode into a corrosion solution II at 25 ℃ to ensure that the electrolytic corrosion surface of the sample is completely immersed in the corrosion solution, turning on the direct current power supply, and regulating the voltage to ensure that the corrosion current density of the metal matrix at the exposed part of the corrosion sample reaches 2A/cm 2 The electrolysis time is 16s, and then the sample is taken out, washed in alcohol and dried;
(4) The interface of diamond and aluminum substrate was observed under a scanning electron microscope, and the result is shown in fig. 4.
As can be seen from FIG. 4, al 4 C 3 Adhesion of phase and silicon phase to diamond surface, wherein Al 4 C 3 The phases are selectively unevenly distributed on different surfaces of the diamond. Since the impregnation temperature of this example was high (750 ℃), al 4 C 3 The phase size is significantly increased and densely distributed on the diamond surface, while the silicon phase distribution is intermediate between example 1 and example 2. Therefore, the corrosive and the inspection method thereof can conveniently and effectively inspect the interface structure of the diamond/aluminum-silicon composite material.
Comparative example 1
(1) Preparing an electrolytic corrosion sample:
exactly the same as in example 2.
(2) The preparation of the corrosive agent and the corrosion method are as follows:
reference is made to the corrosives and inspection methods for diamond/pure Aluminum composite interface display in the i.e. monje paper (i.e. monje, aluminum/diamond composites: A preparative method to characterize reactivity and selectivity at the interface, scripta Materialia 66 (2012) 789-792):
a. etching agent: taking a small amount of deionized water in a beaker, slowly adding 10mL of nitric acid with the mass percent of 68% into the beaker, stirring by using a glass rod to uniformly mix the nitric acid and the nitric acid, adding the deionized water, mixing and fixing the volume to 100mL.
b. Electrochemical corrosion: connecting the corrosion sample with the positive electrode of a direct current power supply, connecting the platinum electrode plate with the negative electrode, then putting the positive electrode and the negative electrode into a corrosion solution at 25 ℃ to ensure that the electrolytic corrosion surface of the sample is completely immersed in the corrosion solution, turning on the direct current power supply, and regulating the voltage to ensure that the corrosion current density of the metal matrix at the exposed part of the corrosion sample reaches 2A/cm 2 The electrolysis time is 2.5min, and then the sample is taken out, washed in alcohol and dried;
c. the interface of diamond and aluminum substrate was observed under a scanning electron microscope, and the result is shown in fig. 5.
As can be seen from FIG. 5, al is not visible on the diamond surface 4 C 3 The phase exists, only densely distributed corrosion pits are seen, which should be interface reactant Al 4 C 3 Pits left after the phase is etched away or falls off. The silicon phase particles were visible on the diamond surface, but were slightly smaller in size than in example 2, indicating that the silicon particles were also subject to some erosion.
As can be seen from comparative analysis of electrolytic corrosion effect graphs of diamond/aluminum silicon composite material interfaces of three examples, al increases with the infiltration temperature 4 C 3 The particles are coarsened gradually, and the distribution at the interface is changed from sparse to dense gradually; as the silicon content in the aluminum-silicon alloy increases, the number of silicon phases on the diamond surface increases gradually. The method can better detect the interface difference of the diamond/aluminum silicon composite materials prepared by different infiltration temperatures and different silicon contents, and provides an effective detection means for the research and production of the composite materials.
Claims (5)
1. The etchant for inspecting the diamond/aluminum-silicon composite material interface is characterized by comprising an etching solution I and an etching solution II, wherein the etching solution I comprises nitric acid, glycerol and water; the corrosion solution II comprises hydrofluoric acid, hypophosphorous acid, glycerol and water; in the corrosion solution I, each 100mL of solution comprises 10-12 mL of nitric acid, 8-10 mL of glycerol and the balance of water; the mass fraction of the nitric acid is 65-70%; each 100mL of solution in the corrosion solution II comprises 5-7 mL of hydrofluoric acid, 7-10 mL of hypophosphorous acid, 8-10 mL of glycerol and the balance of water; the mass fraction of the hydrofluoric acid is 35-40%; and the mass fraction of the hypophosphorous acid is 80-85%.
2. A method of using the etchant of claim 1, comprising the steps of:
(1) Processing the diamond/aluminum silicon composite material sample into a sheet sample, polishing, cleaning and drying;
(2) Connecting the corrosion sample with the positive electrode of a direct current power supply, connecting the platinum electrode with the negative electrode, putting the positive electrode and the negative electrode into a corrosion solution I, starting the direct current power supply to start electrolytic corrosion, taking out the sample, cleaning and drying;
(3) Connecting the sample in the step (2) with the positive electrode of a direct current power supply, connecting a platinum electrode with a negative electrode, putting the positive electrode and the negative electrode into an etching solution II, starting the direct current power supply to start electrolytic etching, taking out the sample, and cleaning and drying the sample in alcohol;
(4) The interface of diamond and aluminum substrate and its reaction products were observed under a scanning electron microscope.
3. The method of claim 2, wherein the diamond/aluminum silicon composite material in step (1) comprises 5-9wt% of silicon in the matrix, and the balance being aluminum.
4. The method of using the etchant as defined in claim 2, wherein the etching solution I in step (2) is electrolytically etched at 25 ℃The current density was 2A/cm 2 The electrolysis time is 10-14 s.
5. The method of using the etchant according to claim 2, wherein the etching current density of electrolytic etching is 2A/cm at a temperature of 25℃for the etching solution II in the step (3) 2 The electrolysis time is 16-20 s.
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| CN101935863A (en) * | 2009-06-30 | 2011-01-05 | 比亚迪股份有限公司 | Aluminum alloy electrolytic polishing solution, preparation method and aluminum alloy electrolytic polishing method |
| CN113088975A (en) * | 2021-03-26 | 2021-07-09 | 西安建筑科技大学 | Metallographic corrosive agent and corrosion method for aluminum/titanium/nickel/stainless steel composite material |
| CN113358645A (en) * | 2021-05-12 | 2021-09-07 | 东南大学 | Etching agent suitable for displaying austenite grains of low-carbon low-alloy steel and display method thereof |
| CN114318341A (en) * | 2021-12-16 | 2022-04-12 | 东风汽车集团股份有限公司 | Aluminum alloy metallographic corrosion method and metallographic corrosion agent thereof |
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| CN101935863A (en) * | 2009-06-30 | 2011-01-05 | 比亚迪股份有限公司 | Aluminum alloy electrolytic polishing solution, preparation method and aluminum alloy electrolytic polishing method |
| CN113088975A (en) * | 2021-03-26 | 2021-07-09 | 西安建筑科技大学 | Metallographic corrosive agent and corrosion method for aluminum/titanium/nickel/stainless steel composite material |
| CN113358645A (en) * | 2021-05-12 | 2021-09-07 | 东南大学 | Etching agent suitable for displaying austenite grains of low-carbon low-alloy steel and display method thereof |
| CN114318341A (en) * | 2021-12-16 | 2022-04-12 | 东风汽车集团股份有限公司 | Aluminum alloy metallographic corrosion method and metallographic corrosion agent thereof |
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