CN107931762B - Method for preparing copper anti-scaling micro-nano composite structure layer by electric spark machining - Google Patents
Method for preparing copper anti-scaling micro-nano composite structure layer by electric spark machining Download PDFInfo
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- CN107931762B CN107931762B CN201711095529.6A CN201711095529A CN107931762B CN 107931762 B CN107931762 B CN 107931762B CN 201711095529 A CN201711095529 A CN 201711095529A CN 107931762 B CN107931762 B CN 107931762B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention discloses a method for preparing a copper anti-scaling micro-nano composite structure layer by electric spark machining, which is characterized in that a copper block is arranged on a clamp of an electric spark forming machine to ensure that the copper block is fully contacted with the clamp; adjusting the spraying direction of an electric spark machining liquid nozzle to point to the surface of the copper block, forming an angle range of 2-15 degrees with the surface of the copper block, and setting electric spark machining parameters; and starting an electric spark forming machine to process the surface of the copper block, wherein the processing depth is 1-2 mm, and macroscopic electric erosion characteristic structures are uniformly distributed on the surface of the copper block to obtain the copper anti-scaling micro-nano composite structure layer. The method is simple and convenient, the copper anti-scaling micro-nano composite structure layer can be prepared only by one processing procedure, the electric spark processing liquid can be recycled for continuous use, the pollution of the processing waste liquid to the environment is reduced, and the additional expenditure brought by the waste liquid treatment is reduced.
Description
Technical Field
The invention relates to the field of material surface engineering, in particular to a method for preparing a copper anti-fouling micro-nano composite structure layer by electric spark machining.
Background
The copper-based material is used as a heat exchange surface material, a heat exchange medium is generally tap water or industrial water, and scale is easily generated on the heat exchange surface, so that the heat exchange efficiency of the heat exchange surface is reduced, chemical components of the scale can corrode an attachment area, and the service life of heat exchange equipment is shortened.
In recent years, researchers develop various anti-scale coatings and preparation technologies thereof according to the characteristics of the scale, systematically research the anti-scale mechanism, and discover that low surface energy can influence the adhesion of the scale on the heat exchange surface, reduce the adhesion of the scale on the heat exchange surface and realize the surface anti-scale property. The common preparation technology of the surface anti-fouling coating mainly comprises methods such as chemical vapor deposition, chemical plating, electrochemical deposition, self-assembly technology, sol-gel method, ion implantation method and the like, wherein the methods mainly adopt a chemical method, one or more layers of thin films are prepared on the heat exchange surface through chemical reaction, the thin films have low surface energy, and the attachment of fouling on the heat exchange surface is reduced. However, the chemically prepared anti-fouling coating is affected by the preparation method, and the defects are obvious: firstly, because the heat exchange interface is a heat exchange effect concentration area, the coating is influenced by bubble vibration and heat flow exchange generated in the boiling heat transfer process, the binding force between the coating and a substrate is greatly reduced, the service life of the coating is directly influenced, and the coating after falling off is mixed in a heat exchange medium to cause pollution and harm of secondary dirt deposition; secondly, the components of the anti-scaling coating affect the heat exchange effect, part of the anti-scaling coating takes the high polymer material as one of the components, and the heat conduction performance of the high polymer material is inferior to that of the metal material and part of the non-metal material, so that the heat transfer effect of the anti-scaling coating is reduced, and although the anti-scaling coating has better anti-scaling performance, the heat transfer efficiency can not meet the requirements of working conditions. Meanwhile, the chemical method for preparing the surface anti-scaling coating is also influenced by preparation scale and environmental pollution, the corresponding preparation cost is higher, and the large-scale industrial production is limited. Therefore, the method has important significance for simply, green and environmentally-friendly preparation of the anti-fouling coating, prolonging the service life of the anti-fouling coating and considering the heat transfer performance.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the method for preparing the copper anti-fouling micro-nano composite structure layer by electric spark machining, which has the advantages of high heat transfer efficiency, environmental friendliness, low cost and simple process.
The purpose of the invention is realized by the following technical scheme:
a method for preparing a copper anti-scaling micro-nano composite structure layer by electric spark machining comprises the following steps: mounting the copper block on a clamp of an electric spark forming machine to ensure that the copper block is in full contact with the clamp; adjusting the spraying direction of an electric spark machining liquid nozzle to point to the surface of the copper block, forming an angle range of 2-15 degrees with the surface of the copper block, and setting electric spark machining parameters; and starting an electric spark forming machine to process the surface of the copper block, wherein the processing depth is 1-2 mm, and macroscopic electric erosion characteristic structures are uniformly distributed on the surface of the copper block to obtain the copper anti-scaling micro-nano composite structure layer.
The copper block is cut into small blocks with the length of 10-20 mm, the width of 10-20 mm and the height of 3-10 mm.
The electric spark machining liquid is an electric spark machining liquid which is sold in the market conventionally, and the physical and chemical indexes of the electric spark machining liquid are as follows: the flash point (closed) is more than 80 ℃, and the kinematic viscosity (40 ℃) range is 1.3-2.2 mm2·s-1The pour point is less than-15 ℃, and the acid value ranges from 0.01 to 0.06mgKOH g-1Saybolt colour > +30, aniline point > 85 ℃, aromatics (FIA analysis) < 0.5%, no antioxidant. The electro-discharge machining liquid may also be deionized water.
The electroerosion characteristic structure is that after the electric spark machining is finished, under macroscopic visual observation, nondirectional micro pits and hard convex edges are uniformly distributed on the surface of a machined sample.
The micro-nano composite structure layer is composed of typical micro-topography characteristics of electric spark machining, comprises nano holes, micro pits, re-melting areas, melting beads and thermal stress cracks, and has low surface energy (1.553-6.025 mJ.m)-2) The hydrophobic surface of (1).
The electric spark machining parameters are as follows: the current is 15-20A, the pulse width is 80-100 mus, the duty ratio is 80%, the gap voltage is 40V, and the processing depth is 1-3 mm.
Before processing, carrying out surface pretreatment on the copper block: polishing the surface of the copper block by using 200-600-mesh abrasive paper, and removing surface impurities and an oxidation layer; and then ultrasonically cleaning the copper block by using acetone, absolute ethyl alcohol and deionized water for 5-10 minutes respectively, cleaning residual abrasive dust on the surface, and then drying the surface of the copper block.
After the processing is finished, cleaning the surface of the copper block: and taking the copper block from the fixture, respectively putting the copper block into acetone, absolute ethyl alcohol and deionized water, and ultrasonically cleaning for 5-10 minutes to remove residual electric spark machining liquid and machining chips.
The principle of the invention is as follows: high temperature caused by discharge in the electric spark machining process melts copper-based surface metal, and electric arc generated between electrodes strikes the surface of a copper matrix, so that a series of typical electric spark machining micro-morphology features are formed on the surface of the copper matrix, and the micro-nano composite structure layer comprises nano holes, micro pits, a re-melting area, melting beads, thermal stress cracks and the like. The structural layer is a hydrophobic surface with low surface energy, and the hydrophobic property of the structural layer can effectively prevent the infiltration of a dirt medium and the attachment and growth of dirt crystals. Meanwhile, the microstructure of the surface layer of the matrix is a re-melted structure formed again after high-temperature melting, the density is higher, the corrosion resistance is good, the corrosion damage of a dirt medium to the matrix structure is avoided, and the hydrophobic property of the surface with low surface energy is further protected. The anti-fouling performance of the surface of the copper matrix is effectively improved under the combined action of the anti-fouling adhesion effect of the low surface energy and the corrosion resistance of the compact remelting metal structure.
Compared with the prior art, the invention has the following advantages and effects:
(1) the electric spark machining method is simple and convenient, and the copper anti-fouling micro-nano composite structure layer can be prepared only by one machining process.
(2) The invention does not need various chemical reagents, and the electric spark processing liquid can be recycled for continuous use, thereby reducing the pollution of the processing waste liquid to the environment and reducing the additional expenditure caused by the waste liquid treatment.
(3) The electric spark machining liquid can adopt deionized water, and environment-friendly production is realized.
(4) The electric spark processing method can be matched with a numerical control system to realize the preparation of the copper anti-scaling micro-nano composite structure layer with a large area or a complex profile.
Drawings
FIG. 1 is a scanning electron microscope image of the copper anti-scaling micro-nano composite structure layer of example 1.
FIG. 2 is a contact angle measurement result of the copper anti-scaling micro-nano composite structure layer.
FIG. 3 is a polarization curve of the copper anti-scaling micro-nano composite structure layer and the smooth surface copper block.
FIG. 4 is an impedance spectrogram of the copper anti-scaling micro-nano composite structure layer and the copper block with the smooth surface, and a small frame in the diagram is an enlarged view of the impedance spectrogram of the copper block with the smooth surface.
FIG. 5 shows a smooth surface copper block on CaCl2+NaOH(0.1mol·L-1) Scanning electron micrographs of surface fouling after 72 hours of immersion in the solution.
FIG. 6 shows that the copper scale-resistant micro-nano composite structure layer of example 1 is on CaCl2+NaOH(0.1mol·L-1) Scanning electron micrographs of surface fouling after 72 hours of immersion in the solution.
FIG. 7 shows that the surface of a smooth copper block and a copper anti-scaling micro-nano composite structure layer of the invention are arranged in CaCl2+NaOH(0.1mol·L-1) Surface soil adhesion weight gain curve during 72 hours of soaking in solution.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
Firstly, cutting a copper block sample with the size of 10mm multiplied by 3mm, polishing the surface of the cut copper block with 200, 400 and 600-mesh abrasive paper respectively, removing impurities and oxide skin on the surface, then ultrasonically cleaning the surface for 5 minutes with acetone, absolute ethyl alcohol and deionized water respectively, cleaning residual abrasive dust on the surface, and then drying the copper block with an air duct; secondly, the copper block is arranged on a clamp of an electric spark forming machine, so that the copper block is ensured to be correctly arranged and can be conducted without short circuit, the spraying direction of the electric spark machining liquid is adjusted to point to the surface of the copper block, an included angle of about 10 degrees is formed between the spraying direction and the surface of the copper block, and electric spark machining parameters are set as follows: the current is 20A, the pulse width is 100 mus, the duty ratio is 80%, the gap voltage is 40V, the processing depth is 1mm, and then the processing is started; and when the electric spark is machined to the set depth, the macroscopic electric erosion characteristic structures are uniformly distributed on the surface of the machined sample, and after the electric spark machining is finished, the copper block is taken down, is respectively placed into acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning for 5 minutes, is taken out and is dried. The contact angle of the copper anti-fouling micro-nano composite structure layer is 139 +/-1.5 degrees.
Example 2
Firstly, cutting a copper block sample with the size of 10mm multiplied by 3mm, polishing the surface of the cut copper block with 200, 400 and 600-mesh abrasive paper respectively, removing impurities and oxide skin on the surface, then ultrasonically cleaning the surface for 5 minutes with acetone, absolute ethyl alcohol and deionized water respectively, cleaning residual abrasive dust on the surface, and then drying the copper block with an air duct; secondly, the copper block is arranged on a clamp of an electric spark forming machine, so that the copper block is ensured to be correctly arranged and can be conducted without short circuit, the spraying direction of the electric spark machining liquid is adjusted to point to the surface of the copper block, an included angle of about 10 degrees is formed between the spraying direction and the surface of the copper block, and electric spark machining parameters are set as follows: the current is 15A, the pulse width is 80 mus, the duty ratio is 80%, the gap voltage is 40V, the processing depth is 1mm, and then the processing is started; and when the electric spark is machined to the set depth, the macroscopic electric erosion characteristic structures are uniformly distributed on the surface of the machined sample, and after the electric spark machining is finished, the copper block is taken down, is respectively placed into acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning for 5 minutes, is taken out and is dried. The contact angle of the copper anti-scaling micro-nano composite structure layer is 133 +/-6.4 degrees.
Example 3
Firstly, cutting a copper block sample, wherein the size of the copper block sample is 10mm multiplied by 3mm, polishing the surface of the cut copper block with 200, 400 and 600-mesh abrasive paper respectively, removing impurities and oxide skin on the surface, then ultrasonically cleaning the surface for 10 minutes with acetone, absolute ethyl alcohol and deionized water respectively, cleaning residual abrasive dust on the surface, and then drying the copper block with an air duct; secondly, the copper block is arranged on a clamp of an electric spark forming machine, so that the copper block is ensured to be correctly arranged and can be conducted without short circuit, the spraying direction of the electric spark machining liquid is adjusted to point to the surface of the copper block, an included angle of about 10 degrees is formed between the spraying direction and the surface of the copper block, and electric spark machining parameters are set as follows: the current is 18A, the pulse width is 100 mus, the duty ratio is 80%, the gap voltage is 40V, the processing depth is 2mm, and then the processing is started; and when the electric spark is machined to the set depth, the macroscopic electric erosion characteristic structures are uniformly distributed on the surface of the machined sample, and after the electric spark machining is finished, the copper block is taken down, is respectively placed into acetone, absolute ethyl alcohol and deionized water for ultrasonic cleaning for 10 minutes, is taken out and is dried. The contact angle of the copper anti-scaling micro-nano composite structure layer is 129 +/-2.0 degrees.
Test example
And comparing the copper blocks with the smooth surface as a comparative example, and performing performance comparative analysis on the copper blocks with the copper anti-scaling micro-nano composite structure layer prepared in the embodiment of the invention.
As can be seen from FIG. 1, after the copper surface is subjected to electric spark machining, an obvious electroerosion characteristic structure exists, including an electroerosion pit, a remelting region, a molten bead and a thermal stress crack, wherein the dimension range of the electroerosion pit is from nanometer to micrometer. The electroerosion characteristic structures are uniformly distributed on the surface of the copper to form a micro-nano composite structure layer. The structural layer is a hydrophobic surface with low surface energy.
The contact angle measurement result of the copper anti-fouling micro-nano composite structure layer of the example 1 on deionized water is shown in figure 2, the contact angle result is 139 +/-1.5 degrees, and the surface energy is 2.629 mJ.m-2。
As can be seen from fig. 3, the polarization curve of the copper anti-scaling micro-nano composite structure layer of example 1 is shifted to the positive direction compared with the polarization curve of the copper block with the smooth surface, and the self-corrosion potential is 0.001V; the polarization curve of the copper anti-scaling micro-nano composite structure layer in the embodiment 2 deviates to the positive direction compared with the polarization curve of a copper block with a smooth surface, and the self-corrosion potential is-0.022V; the polarization curve of the copper anti-scaling micro-nano composite structure layer in the example 3 is deviated from the polarization curve of the copper block with the smooth surface to the positive direction, and the self-corrosion potential is 0.007V.
As can be seen from fig. 4, the polarization resistance values of the copper anti-scaling micro-nano composite structure layers of examples 1, 2 and 3 are far greater than that of the copper block with a smooth surface. Therefore, the corrosion resistance of the copper anti-scaling micro-nano composite structure layer prepared by the method is superior to that of a copper block with a smooth surface.
Respectively soaking the copper anti-scaling micro-nano composite structure layers and the copper blocks with smooth surfaces of the examples 1, 2 and 3 in CaCl in different beakers2+NaOH(0.1mol·L-1) In the solution, the sample is taken out and dried at the same time every 8 hours, and then CaCO on the surface of the sample is weighed by an electronic balance3The soil adhesion amount data, the duration of the experiment was 72 hours, and the surface trend curve of the soil adhesion amount with time was plotted, as shown in fig. 7. As can be seen from FIG. 7, the anti-scaling micro-nano composite structure layer of copper and the copper block with the smooth surface of the copper in the example 1 are CaCO within the soaking time3The adhesion amount of dirt on the surface is increased along with the increase of time, but the adhesion amount of the dirt in the example 1 is smaller than that of the smooth surface copper block, and the fluctuation range of the adhesion amount of the dirt is smaller than that of the smooth surface copper block, which shows that the copper anti-dirt micro-nano composite structure layer in the example 1 is anti-dirt than that of the smooth surface copper block. The overall tendency of the surface scale adhesion amount of example 2 is to increase with time, but the increase amount is smaller than that of the smooth surface copper block, and the overall variation tendency of the scale adhesion amount fluctuates less, indicating that the copper scale-resistant composite structure layer of example 2 is more resistant to scale than the smooth surface copper block. The change of the surface dirt adhesion amount of the example 3 is small along with the increase of time, the overall change trend of the dirt adhesion amount is flat, and the dirt adhesion amount is far smaller than that of the smooth surface copper block, which shows that the copper dirt-resistant composite structure layer of the example 3 is more dirt-resistant than that of the smooth surface copper block.
After the experiment, the surface fouling of the copper block of example 1 and the smooth surface was observed by scanning electron microscope, and the results are shown in fig. 5 and fig. 6. As can be seen from fig. 5 and 6, after 72 hoursCaCO with copper block adhered on smooth surface after soaking in dirt solution3The number of crystals is much more than that of the CaCO of the embodiment 1, and the CaCO is attached to the surface of the embodiment 1 in the figure 63The average size of the crystals is small. It can be seen that the scanning electron microscope results shown in fig. 5 and fig. 6 further prove that the anti-scaling performance of the copper anti-scaling micro-nano composite structure layer of the embodiment 1 is good and superior to that of a smooth surface copper block.
Claims (8)
1. A method for preparing a copper anti-scaling micro-nano composite structure layer by electric spark machining is characterized by comprising the following steps: mounting the copper block on a clamp of an electric spark forming machine to ensure that the copper block is in full contact with the clamp; adjusting the spraying direction of an electric spark machining liquid nozzle to point to the surface of the copper block, forming an angle range of 2-15 degrees with the surface of the copper block, and setting electric spark machining parameters; starting an electric spark forming machine to process the surface of the copper block, wherein the processing depth is 1-2 mm, and macroscopic electric erosion characteristic structures are uniformly distributed on the surface of the copper block to obtain a copper anti-scaling micro-nano composite structure layer; the electroerosion characteristic structure is a micro-nano composite structure layer consisting of nano holes, micro pits, a re-melting area, melting beads and thermal stress cracks.
2. The method for preparing the copper anti-scaling micro-nano composite structure layer by electric spark machining according to claim 1, which is characterized in that: the physicochemical indexes of the electric spark machining liquid are as follows: the closed flash point is more than 80 ℃, the kinematic viscosity range at 40 ℃ is 1.3-2.2 mm2·s-1The pour point is less than-15 ℃, and the acid value ranges from 0.01 to 0.06mgKOH g-1Saybolt colour > 30, aniline point > 85 deg.C, FIA analysis aromatics < 0.5%, no antioxidant.
3. The method for preparing the copper anti-scaling micro-nano composite structure layer by electric spark machining according to claim 1, which is characterized in that: the electrical discharge machining liquid is deionized water.
4. The method for preparing the copper anti-scaling micro-nano composite structure layer by electric spark machining according to claim 1, which is characterized in that: the electroerosion characteristic structure is that after the electric spark machining is finished, under macroscopic visual observation, nondirectional micro pits and hard convex edges are uniformly distributed on the surface of a machined sample.
5. The method for preparing the copper anti-scaling micro-nano composite structure layer by electric spark machining according to claim 1, which is characterized in that: the micro-nano composite structure layer is composed of typical micro-topography characteristics of electric spark machining, comprises nano holes, micro pits, a re-melting area, melting beads and thermal stress cracks and has the thickness of 1.553-6.025 mJ.m-2Hydrophobic surfaces of low surface energy.
6. The method for preparing the copper anti-scaling micro-nano composite structure layer by electric spark machining according to claim 1, which is characterized in that: the electric spark machining parameters are as follows: the current is 15-20A, the pulse width is 80-100 mus, the duty ratio is 80%, the gap voltage is 40V, and the processing depth is 1-2 mm.
7. The method for preparing the copper anti-scaling micro-nano composite structure layer by electric spark machining according to claim 1, which is characterized in that: before processing, carrying out surface pretreatment on the copper block: polishing the surface of the copper block by using 200-600-mesh abrasive paper, and removing surface impurities and an oxidation layer; and then ultrasonically cleaning the copper block by using acetone, absolute ethyl alcohol and deionized water for 5-10 minutes respectively, cleaning residual abrasive dust on the surface, and then drying the surface of the copper block.
8. The method for preparing the copper anti-scaling micro-nano composite structure layer by electric spark machining according to claim 1, which is characterized in that: after the processing is finished, cleaning the surface of the copper block: and taking the copper block from the fixture, respectively putting the copper block into acetone, absolute ethyl alcohol and deionized water, and ultrasonically cleaning for 5-10 minutes to remove residual electric spark machining liquid and machining chips.
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| US5648122A (en) * | 1994-09-28 | 1997-07-15 | Ford Motor Company | Using electrical discharge surface preparation for thermal coatings |
| US5818006A (en) * | 1995-12-07 | 1998-10-06 | Ford Global Technologies, Inc. | Surface preparation electrical discharge apparatus and method |
| CN103317198A (en) * | 2013-05-27 | 2013-09-25 | 长春理工大学 | One-step preparation method of metal material surface with super-hydrophobic micro-nano structure |
| CN106270853A (en) * | 2016-09-21 | 2017-01-04 | 河南理工大学 | A kind of processing method of micro structure array |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5648122A (en) * | 1994-09-28 | 1997-07-15 | Ford Motor Company | Using electrical discharge surface preparation for thermal coatings |
| US5818006A (en) * | 1995-12-07 | 1998-10-06 | Ford Global Technologies, Inc. | Surface preparation electrical discharge apparatus and method |
| CN103317198A (en) * | 2013-05-27 | 2013-09-25 | 长春理工大学 | One-step preparation method of metal material surface with super-hydrophobic micro-nano structure |
| CN106270853A (en) * | 2016-09-21 | 2017-01-04 | 河南理工大学 | A kind of processing method of micro structure array |
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