CN111423812B - Preparation process and application of water-based nano coating material and microcrack diagnosis circuit - Google Patents
Preparation process and application of water-based nano coating material and microcrack diagnosis circuit Download PDFInfo
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- CN111423812B CN111423812B CN202010182315.8A CN202010182315A CN111423812B CN 111423812 B CN111423812 B CN 111423812B CN 202010182315 A CN202010182315 A CN 202010182315A CN 111423812 B CN111423812 B CN 111423812B
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- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
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- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
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Abstract
The invention discloses a preparation process and application of a water-based nano coating material and a microcrack diagnosis circuit. With the laser direct patterning + fine grain plating method, a conductive path width of 100 microns or less can be obtained. The invention aims to take out the influence of other fillers, improve the precision of the laser direct imaging circuit and enable the circuit to reach the preset mechanical property. The added laser direct imaging workpiece is sprayed with the water-based nano coating in advance, so that the influence of other fillers on the processing performance, the mechanical property and the later laser processing performance of the material is avoided, and the quality of the workpiece is greatly improved; the prepared coating has good adhesive force, salt fog resistance, high temperature and humidity resistance and cold and hot shock resistance, and the diagnosis circuit has good adhesive force and electric conductivity.
Description
Technical Field
The invention belongs to the technical field of surface microcrack diagnosis, and particularly relates to a preparation process and application of a water-based nano coating material and a microcrack diagnosis circuit.
Background
At present, for diagnosing surface microcracks, a mode of embedding fine metal wires in materials is mainly adopted. The disadvantages of this solution are 1: the strength of the existing thin metal wire is superior to that of a base material, so that the thin metal wire is not always broken when the material is cracked. The error rate reaches about 40% by the detection mode of the conductive signal and the RF signal. 2. In order to ensure that the base material is broken and the thin metal wire is broken synchronously, the diameter of the metal wire is required to be thin, and the preparation of the metal wire and the implantation of the metal wire into the base material are difficult to operate. When the metal wire is used as a filling material, the broken metal wire on the surface of the product is not always broken, and misdiagnosis can be caused. Meanwhile, the production precision of the laser direct patterning line in the actual production process is not high (due to the doping of other fillers), the correspondingly produced line is relatively uneven, and the mechanical property of the line is poor.
A special active catalyst is used in the Laser Direct Patterning (LDP) method. The laser draws a circuit pattern on the surface of the workpiece, the light beam passes through the circuit pattern to cause micro-roughness on the surface, and the path of the laser is also the exposed position of the active catalytic center of the metal. These active catalytic sites are the crystallization nuclei for the next electroless plating process. Other electroless plating methods that may be used include, but are not limited to, copper, gold, nickel, silver, zinc, tin, chromium, cadmium, and the like.
In the actual processing process, the uniformity of the particles dispersed in the material determines the thickness uniformity of the line of the LDP technology, and the dispersion performance simultaneously influences the processing performance of the material. Therefore, it is necessary to introduce special processing aids and to use special treatment methods, and furthermore, since the metal oxides usually undergo molecular chain breakage in the heated state, the final mechanical properties of the material are affected. It is therefore necessary to introduce suitable adjuvants to inhibit thermal degradation of the system. While controlling the amount of addition, excessive amounts of addition can result in changes in other properties of the material.
In the actual processing process, besides the requirement of meeting the material processing performance, the formula design needs to add a large amount of additives in the formula due to the difference of the final use requirements of the product so as to meet other performance indexes: such as increasing the dielectric value of the material, increasing its combustion-supporting properties, adding other pigments to improve the color requirements, adding fibers to improve dimensional stability, etc. This is generally such that it contains a large amount of fillers of inorganic type.
The conventional method does not carry out any treatment on the added laser direct patterning material to directly fill the material, so that the using effect of the material is influenced, and the formulation involved in practical application usually contains other fillers, and the additive effects cause the processability and mechanical properties of the formulation material and the later laser processability to be reduced. Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
The invention aims to provide a preparation process and application of a water-based nano coating material and a microcrack diagnosis circuit, so as to solve the problems in the background technology.
One of the purposes of the invention is to provide a water-based nano coating material, which is prepared from a solid phase and a liquid phase according to the mass ratio of 1: 1, the solid phase consists of the following raw materials: 30-45 wt% of kaolin, 10-15 wt% of cobalt blue, 20-38 wt% of quartz powder, 8-20 wt% of iron oxide red, 3-15 wt% of alumina short fiber and 3-10 wt% of filler; the liquid phase consists of 50-60 wt% of silica hybrid and 40-50 wt% of PAI; the filler is titanium dioxide;
preferably, the aqueous nano-coating material is prepared from a solid phase and a liquid phase according to a mass ratio of 1: 1, the solid phase consists of the following raw materials: 35 wt% of kaolin, 15 wt% of cobalt blue, 27 wt% of quartz powder, 12 wt% of iron oxide red, 5wt% of alumina short fiber and 6 wt% of filler; the liquid phase consists of 55 wt% of silica hybrid and 45 wt% of PAI; the filler is titanium dioxide;
controlling the mass ratio of the solid phase to the liquid phase to be 1: 1. the composition of the solid phase component and the composition of the liquid phase component enable the prepared coating to be firmer, and the coating has better adhesive force, high temperature resistance, high humidity resistance and salt fog resistance.
The invention also aims to provide a preparation process of the microcrack diagnosis circuit based on the water-based nano coating, wherein the water-based nano coating material is the water-based nano coating material, and the preparation process of the microcrack diagnosis circuit comprises the following steps:
step 1, taking a water-based nano coating material according to a ratio, mixing the water-based nano coating material, and stirring for 5-10 hours at a rotating speed: 20-50 rpm; temperature: normal temperature;
step 3, carrying out laser direct graphical processing on the workpiece after the spraying is finished;
step 4, placing the workpiece treated in the step 3 into ultrasonic dust removal equipment for treatment for 5-15 minutes, wherein the water dripping time is 20-30 seconds, and the treatment is carried out in an environment of 50-60 ℃;
step 5, subjecting the workpiece subjected to ultrasonic treatment to two washing treatments at normal temperature, wherein the washing treatment lasts for 1-2 minutes, the dripping time lasts for 15-30 seconds, and air stirring is adopted in the washing treatment process;
step 6, carrying out copper impact treatment on the workpiece washed in the step 5 at the temperature of 50-62 ℃, wherein the treatment time is 10-30 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 7, carrying out two washing treatments on the workpiece treated in the step 6 at a normal temperature, wherein the washing treatment time is 0.5-1 minute, the dripping time is 20-30 seconds, and air stirring is adopted in the washing treatment process;
step 8, carrying out chemical thick copper plating treatment on the workpiece treated in the step 7 at the temperature of 50-56 ℃, wherein the treatment time is 60-180 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 9, carrying out three pure water washing treatments on the workpiece treated in the step 8 at normal temperature, wherein the water washing treatment time is 30 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the water washing treatment process;
step 10, performing pre-dipping treatment on the workpiece treated in the step 9 through a middle conversion hanger at normal temperature, wherein the treatment time is 3-5 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the pre-dipping treatment process;
step 11, performing nickel pre-activation treatment on the workpiece treated in the step 10 at the temperature of 32-38 ℃, wherein the treatment time is 5-10 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts mechanical circulation;
step 12, carrying out two times of pure water washing treatment on the workpiece treated in the step 11 at normal temperature, wherein the water washing treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the water washing treatment process;
step 13, carrying out post-dipping treatment on the workpiece treated in the step 12 in a normal temperature environment, wherein the treatment time is 2-5 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 14, carrying out three times of pure water washing treatment on the workpiece treated in the step 13 at normal temperature, wherein the treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the treatment process;
step 15, carrying out chemical nickel treatment on the workpiece treated in the step 14 at the temperature of 60-85 ℃, wherein the treatment time is 10-25 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 16, performing two times of pure water washing treatment on the workpiece treated in the step 15 at normal temperature, wherein the treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the treatment process;
and step 17, carrying out nickel-gold protection treatment on the workpiece treated in the step 16 at the temperature of 35-45 ℃, wherein the treatment time is 3-8 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts mechanical circulation.
Step 18, carrying out three times of pure water washing treatment on the workpiece treated in the step 17 at normal temperature, wherein the treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the treatment process;
and 19, carrying out hot water washing treatment on the workpiece treated in the step 18 at the temperature of 60-70 ℃, wherein the treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the treatment process.
According to the process, the rupture strength of the composite deposited metal circuit prepared by the invention is not more than that of the matrix material, and the conductivity of the composite deposited metal circuit is not less than 1.6510-8Ω m -1.75 ×10-8Omega m; composite deposited metal lines 3M 610 tape test hundred grid area, vertical drawing 6 times, no shedding.
Further, the thickness distribution of the three-layer coating is respectively as follows: bottom layer: 6-12 microns; middle layer: 12-20 microns; surface layer: 15-20 microns.
Further, the bottom layer is an adhesion promoting layer, and the curing temperature is 75-85 ℃ and the time is 20-40min in the spraying process; the middle layer is a colored paint layer, the curing temperature is 80-120 ℃ in the spraying process, and the time is 1.5-2.5 hours; the surface layer is an appearance protective layer, and the curing temperature is 80-120 ℃ and the time is 1.5-2.5 hours in the spraying process.
The thickness of the coating is set to three layers, the spraying process is adopted in the spraying process, and each layer has the thickness as described in the invention, so that the coating has good adhesive force and high temperature, high humidity and salt mist resistance, and meanwhile, the cold and hot impact performance of the coating is greatly improved.
Furthermore, the laser processing parameters in the laser direct patterning method are filling distance <50 microns, scanning frequency 40-100 kilohertz, scanning speed 1000-: 1064 nm.
Further, the solution used in the impact copper treatment process of step 6 comprises the following components: 200 parts of copper complexing agent 150-; wherein, the copper complexing agent is EDTA and sodium potassium tartrate according to the weight ratio of 1: 1.
Further, the solution used in the impact copper treatment process of step 6 comprises the following components: 180 parts of copper complexing agent, 35 parts of copper sulfate, 1.5 parts of methanol, 32 parts of sodium hydroxide, 16 parts of formaldehyde and 750 parts of deionized water; wherein, the copper complexing agent is EDTA and sodium potassium tartrate according to the weight ratio of 1: 1.
Further, the step 6 of preparing the solution used in the impact copper treatment process comprises the following steps:
a) adding 350-500 parts of deionized water into a prepared clean plating bath;
b) starting air stirring, and adding 150 and 200 parts of copper complexing agent;
c) adding 20-40 parts of copper sulfate;
d) adding 1-5 parts of methanol;
e) adding 25-35 parts of sodium hydroxide;
f) then adding 350-500 parts of deionized water to the liquid preparation amount;
g) heating the plating tank to 54-62 ℃;
h) adding 12-18 parts of formaldehyde;
i) and (3) heating to an operating condition, analyzing the concentrations of the complexing agent, copper ions, formaldehyde, sodium hydroxide and the complexing agent, and adjusting the concentrations of the complexing agent in the process range for feeding and trial production.
The agents are added according to the sequence strictly and are fully and uniformly mixed, concentration polarization is avoided, and the reducing agent formaldehyde is added after the temperature reaches the working temperature.
Further, the process range of the solution used in the impact copper treatment process in the step 6 is that the copper concentration is 2.0-3.0g/L, the alkali concentration is 7.0-11.0g/L, the total chelating agent is 32-40g/L, the formaldehyde concentration is 3.0-5.0g/L, the temperature is 55-62 ℃, the time is 10-30min, and the thickness is controlled to be 1-3 μm.
Further, the process range of the solution used in the copper-strike treatment process in step 6 is that the copper concentration is 2.5g/L, the alkali concentration is 9.5g/L, the total chelating agent is 34g/L, the formaldehyde concentration is 4.0g/L, the temperature is 58 ℃, the time is 20min, and the thickness is controlled to be 2 μm.
Further, the solution used in the chemical thick copper plating treatment process in the step 8 comprises the following components: 180 portions of copper complexing agent 120, 20 to 25 portions of copper sulfate, 0.4 to 0.8 portion of methanol, 20 to 25 portions of sodium hydroxide, 8 to 12 portions of formaldehyde and 1000 portions of deionized water 700; wherein, the copper complexing agent is EDTA and sodium potassium tartrate according to the weight ratio of 1: 1.
Further, the solution used in the chemical thick copper plating treatment process in the step 8 comprises the following components: 150 parts of copper complexing agent, 22 parts of copper sulfate, 0.6 part of methanol, 22 parts of sodium hydroxide, 10 parts of formaldehyde and 790 parts of deionized water; wherein, the copper complexing agent is EDTA and sodium potassium tartrate according to the weight ratio of 1: 1.
The plating layer prepared by strictly following the process steps and the process range has better adhesive force, high temperature resistance, high humidity resistance, salt fog resistance and cold and hot shock resistance.
Further, the preparation method of the solution used in the process of the step 8 of electroless thick copper plating treatment comprises the following steps:
a) adding 350-500 parts of deionized water into a prepared clean plating bath;
b) starting air stirring, and adding 120 and 180 parts of copper complexing agent;
c) adding 20-25 parts of copper sulfate;
d) adding 0.4-0.8 part of methanol;
e) adding 20-25 parts of sodium hydroxide;
f) then adding 350-500 parts of deionized water to the liquid preparation amount;
g) heating the plating tank to 50-56 ℃;
h) adding 8-12 parts of formaldehyde;
i) and (3) heating to an operating condition, analyzing the concentrations of the complexing agent, copper ions, formaldehyde, sodium hydroxide and the complexing agent, and adjusting the concentrations of the complexing agent in the process range for feeding and trial production.
The agents are added according to the sequence strictly and are fully and uniformly mixed, concentration polarization is avoided, and the reducing agent formaldehyde is added after the temperature reaches the working temperature.
Furthermore, the process range of the solution used in the process of electroless thick copper plating treatment in the step 8 is that the copper concentration is 2.0-3.0g/L, the alkali concentration is 4.5-5.5g/L, the total chelating agent is 22-32g/L, the formaldehyde concentration is 4.5-5.5g/L, the temperature is 50-56 ℃, and the time is 1-3 hours.
Further, the process range of the solution used in the electroless thick copper plating treatment process in the step 8 is that the copper concentration is 2.2g/L, the alkali concentration is 5g/L, the total chelating agent is 25g/L, the formaldehyde concentration is 5g/L, the temperature is 53 ℃, and the time is 2 hours.
The plating layer prepared by strictly following the process steps and the process range has better adhesive force, high temperature resistance, high humidity resistance, salt fog resistance and cold and hot shock resistance.
The invention also aims to provide an application of the preparation process of the microcrack diagnosis circuit, which is applied to the surface of a bearing.
The invention has the technical effects and advantages that:
1. the invention adopts the water-based nano coating material which can be metalized by laser and is developed independently, and the surface of the material is activated at the position where the conductive path is to be arranged by moving the laser beam on the surface of the product. With the laser direct patterning + fine grain plating method, a conductive path width of 100 microns or less can be obtained. The invention aims to take out the influence of other fillers, improve the precision of the laser direct imaging circuit and enable the circuit to reach the preset mechanical property. The added laser direct imaging workpiece is sprayed with the water-based nano coating in advance, so that the influence of other fillers on the processing performance, the mechanical property and the later laser processing performance of the material is avoided, and the quality of the workpiece is greatly improved;
2. the surface microcrack diagnosis circuit matched with the breaking strength of the base material adopts the water-based nano coating material capable of being activated by laser to protect the whole material surface, ensures that the base material is not influenced by a medicament system in the circuit manufacturing, can obtain a required microcrack diagnosis circuit pattern in an activation area on the surface of the water-based nano coating in a laser activation mode, and is used as a crack diagnosis circuit after passing through a fine-grain Cu-Ni-Au composite metallization deposition layer.
Drawings
FIG. 1 is a schematic structural diagram of an application of the preparation process of the microcrack diagnosis circuit based on the water-based nano coating on the bearing surface;
in the figure: 1 bearing body, 2 diagnostic circuit.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to fig. 1 in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
an aqueous nanocoating material, comprising a solid phase and a liquid phase in a mass ratio of 1: 1, the solid phase consists of the following raw materials: 35 wt% of kaolin, 15 wt% of cobalt blue, 27 wt% of quartz powder, 12 wt% of iron oxide red, 5wt% of alumina short fiber and 6 wt% of filler; the liquid phase consists of 55 wt% of silica hybrid and 45 wt% of PAI; the filler is titanium dioxide.
Example 2:
a preparation process of a microcrack diagnosis circuit based on an aqueous nano-coating, wherein the aqueous nano-coating material is the aqueous nano-coating material, and the preparation process of the microcrack diagnosis circuit comprises the following steps:
step 1, taking a water-based nano coating material according to a ratio, mixing the water-based nano coating material, and stirring for 8 hours at a rotating speed: 30 revolutions per minute; temperature: normal temperature;
step 3, carrying out laser direct graphical processing on the workpiece after the spraying is finished;
step 4, placing the workpiece processed in the step 3 into ultrasonic dust removal equipment for processing for 5-15 minutes, wherein the dripping time is 25 seconds, and the processing is carried out in an environment of 55 ℃;
step 5, subjecting the workpiece subjected to ultrasonic treatment to two washing treatments at normal temperature, wherein the washing treatment lasts for 1 minute, the dripping time lasts for 25 seconds, and air stirring is adopted in the washing treatment process;
step 6, carrying out copper impact treatment on the workpiece washed in the step 5 at the temperature of 55 ℃, wherein the treatment time is 20 minutes, the water dripping time is 25 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 7, performing two washing treatments on the workpiece treated in the step 6 at normal temperature, wherein the washing treatment time is 0.5 minute, the dripping time is 25 seconds, and air stirring is adopted in the washing treatment process;
step 8, carrying out chemical thick copper plating treatment on the workpiece treated in the step 7 at the temperature of 55 ℃, wherein the treatment time is 100 minutes, the water dripping time is 25 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 9, under the normal temperature state, the workpiece after being processed in the step 8 is subjected to three pure water washing treatments, wherein the water washing treatment time is 30 minutes, the water dripping time is 25 seconds, and air stirring is adopted in the water washing treatment process;
step 10, performing pre-dipping treatment on the workpiece treated in the step 9 by using a middle conversion hanger at normal temperature, wherein the treatment time is 4 minutes, the water dripping time is 25 seconds, and air stirring is adopted in the pre-dipping treatment process;
11, performing nickel pre-activation treatment on the workpiece treated in the step 10 at the temperature of 35 ℃, wherein the treatment time is 8 minutes, the water dripping time is 25 seconds, and the treatment process adopts mechanical circulation;
step 12, carrying out two times of pure water washing treatment on the workpiece treated in the step 11 at normal temperature, wherein the water washing treatment time is 1 minute, the water dripping time is 25 seconds, and air stirring is adopted in the water washing treatment process;
step 13, carrying out post-dipping treatment on the workpiece treated in the step 12 in a normal temperature environment, wherein the treatment time is 3 minutes, the water dripping time is 25 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 14, performing three times of pure water washing treatment on the workpiece treated in the step 13 at normal temperature, wherein the treatment time is 1 minute, the water dripping time is 25 seconds, and air stirring is adopted in the treatment process;
step 15, carrying out chemical nickel treatment on the workpiece treated in the step 14 at 83 ℃, wherein the treatment time is 20 minutes, the water dripping time is 25 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 16, performing two times of pure water washing treatment on the workpiece treated in the step 15 at normal temperature, wherein the treatment time is 1 minute, the water dripping time is 25 seconds, and air stirring is adopted in the treatment process;
and step 17, performing nickel-gold protection treatment on the workpiece treated in the step 16 at the temperature of 40 ℃, wherein the treatment time is 5 minutes, the water dripping time is 25 seconds, and the treatment process adopts mechanical circulation.
Step 18, carrying out three times of pure water washing treatment on the workpiece treated in the step 17 at normal temperature, wherein the treatment time is 2 minutes, the water dripping time is 25 seconds, and air stirring is adopted in the treatment process;
step 19, carrying out hot water washing treatment on the workpiece treated in the step 18 at the temperature of 5 ℃, wherein the treatment time is 2 minutes, the water dripping time is 25 seconds, and air stirring is adopted in the treatment process; .
The thickness distribution of the three layers of coatings is respectively as follows: bottom layer: 8 microns; middle layer: 15 microns; surface layer: 18 microns.
The bottom layer is an adhesion promoting layer, and the curing temperature is 80 ℃ and the time is 30min in the spraying process; the middle layer is a colored paint layer, and the curing temperature is 100 ℃ and the time is 2 hours in the spraying process; the surface layer is an appearance protective layer, and the curing temperature is 100 ℃ and the time is 2 hours in the spraying process.
The laser processing parameters in the laser direct imaging method are that the filling space is less than 50 microns, the scanning frequency is 80 kilohertz, the scanning speed is 1500 millimeters/second, the power is 8 watts, and the laser wavelength is as follows: 1064 nm.
Step 6 the impact copper treatment process uses a solution comprising the following components: 180 parts of copper complexing agent, 35 parts of copper sulfate, 1.5 parts of methanol, 32 parts of sodium hydroxide, 16 parts of formaldehyde and 750 parts of deionized water; wherein, the copper complexing agent is EDTA and sodium potassium tartrate according to the weight ratio of 1: 1.
The preparation method of the solution used in the impact copper treatment process in the step 6 comprises the following steps:
a) 325 parts of deionized water is added into the prepared clean plating bath;
b) starting air to stir, and adding 180 parts of copper complexing agent;
c) adding 30 parts of copper sulfate;
d) 1.5 parts of methanol are added;
e) 32 parts of sodium hydroxide are added;
f) then 325 parts of deionized water is added to the solution preparation amount;
g) heating the plating bath to 58 ℃;
h) adding 16 parts of formaldehyde;
i) and (3) heating to an operating condition, analyzing the concentrations of the complexing agent, copper ions, formaldehyde, sodium hydroxide and the complexing agent, and adjusting the concentrations of the complexing agent in the process range for feeding and trial production.
The process range of the solution used in the copper impacting treatment process in the step 6 is that the copper concentration is 2.5g/L, the alkali concentration is 9.5g/L, the total chelating agent is 34g/L, the formaldehyde concentration is 4.0g/L, the temperature is 58 ℃, the time is 20min, and the thickness is controlled to be 2 μm.
The solution used in the chemical thick copper plating treatment process in the step 8 comprises the following components: 150 parts of copper complexing agent, 22 parts of copper sulfate, 0.6 part of methanol, 22 parts of sodium hydroxide, 10 parts of formaldehyde and 790 parts of deionized water; wherein, the copper complexing agent is EDTA and sodium potassium tartrate according to the weight ratio of 1: 1.
The preparation method of the solution used in the chemical thick copper plating treatment process in the step 8 comprises the following steps:
a) 345 parts of deionized water is added into the prepared clean plating bath;
b) starting air to stir, and adding 150 parts of copper complexing agent;
c) adding 22 parts of copper sulfate;
d) 0.6 part of methanol was added;
e) 22 parts of sodium hydroxide are added;
f) adding 345 parts of deionized water to the solution preparation amount;
g) heating the plating bath to 53 ℃;
h) adding 10 parts of formaldehyde;
i) and (3) heating to an operating condition, analyzing the concentrations of the complexing agent, copper ions, formaldehyde, sodium hydroxide and the complexing agent, and adjusting the concentrations of the complexing agent in the process range for feeding and trial production.
Further, the process range of the solution used in the electroless thick copper plating treatment process in the step 8 is that the copper concentration is 2.2g/L, the alkali concentration is 5g/L, the total chelating agent is 25g/L, the formaldehyde concentration is 5g/L, the temperature is 53 ℃, and the time is 2 hours.
Example 3:
the application of the preparation process of the microcrack diagnosis circuit based on the water-based nano coating is the application on the surface of a bearing; as shown in fig. 1, a bearing is used as a workpiece, the preparation process of the microcrack diagnosis line is adopted, and the bearing comprises a bearing main body 1 and a diagnosis line 2; producing a high-quality composite deposited metal diagnosis circuit, wherein the fracture strength of the high-quality composite deposited metal diagnosis circuit is close to the fracture strength of the bearing but not more than the fracture strength of the bearing body;
comparative example 1
Comparative example 1 an aqueous nanocoating preparation process as in example 2 differs from example 2 in that a solid to liquid ratio of 1.5: 1;
comparative example 2
Comparative example 2 aqueous nanocoating preparation process as in example 2, differing from example 2 in that the liquid phase is PAI only;
comparative example 3
Comparative example 3 the process for preparing an aqueous nanocoating as in example 2 differs from example 2 in that the liquid phase is PAI only in an amount of 70wt%, and the silica hybrid in an amount of 30 wt%;
comparative example 4
Comparative example 4 a plating preparation process was performed as in example 2, except that the copper concentration was 3.5 g/L;
comparative example 5
Comparative example 5 a plating preparation process was performed as in example 2, except that the working temperature was 65 ℃;
comparative example 6
Comparative example 6 the plating preparation process was as in example 2 except that the working temperature was 45 ℃;
the following table respectively carries out comparison performance tests on the conductivity and adhesion tests of the water-based nano coating, the plating layer and the diagnosis line;
performance test of Water-based Nano coating (Table 1)
Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
Adhesion (3M 610 tape test hundred grid area, vertical pull 6 times) | Without falling off | Slight detachment | Slight detachment | Slight detachment |
Neutral salt spray test of 96 hours 5wt% NaCl | No change on the surface, no appearance Bubbling and no shedding | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off |
96 hours 85wt% relative humidity, 85 ℃ high temperature high humidity test Test (experiment) | No change on the surface, no appearance Bubbling and no shedding | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off |
240 hours 85wt% relative humidity, 85 ℃ to-40 ℃ cold Thermal shock test, temperature rise rate not less than 30 deg.C/s | No change on the surface, no appearance Bubbling and no shedding | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off |
As can be seen from Table 1, the coatings prepared by the present invention have more excellent adhesion, salt spray resistance, high temperature and high humidity resistance, and cold and hot impact resistance, compared to comparative examples 1-3.
Bearing coating performance test (Table 2)
Example 2 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
Neutral salt spray test of 96 hours 5wt% NaCl | No change on the surface, no appearance Bubbling and no shedding | Light surfaceMicro-emergence Bubble and no falling off | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off |
96 hours 85wt% relative humidity, 85 ℃ high temperature high humidity test Test (experiment) | No change on the surface, no appearance Bubbling and no shedding | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off |
240 hours 85wt% relative humidity, 85 ℃ to-40 ℃ cold Thermal shock test, temperature rise rate not less than 30 deg.C/s | No change on the surface, no appearance Bubbling and no shedding | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off | Surface appeared slightly Bubble and no falling off |
As can be seen from Table 2, the coating prepared by the invention has better adhesive force, salt fog resistance, high temperature and high humidity resistance and cold and hot impact resistance compared with the comparative ratio of 4-6.
Comparative examples 1 to 6 were each prepared as a microcrack diagnosis circuit on the bearing surface, and the conductivity and adhesion of the bearing diagnosis circuit were tested (Table 3)
As can be seen from Table 3, the diagnostic circuit prepared by the present invention has more excellent adhesion and conductivity than the comparative examples 1 to 6.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. An aqueous nano-coating material, characterized in that: the water-based nano coating material is prepared from a solid phase and a liquid phase according to a mass ratio of 1: 1, the solid phase consists of the following raw materials: 30-45 wt% of kaolin, 10-15 wt% of cobalt blue, 20-38 wt% of quartz powder, 8-20 wt% of iron oxide red, 3-15 wt% of alumina short fiber and 3-10 wt% of filler; the liquid phase consists of 50-60 wt% of silica hybrid and 40-50 wt% of PAI, and the filler is titanium dioxide.
2. The aqueous nanocoating material of claim 1, wherein: the water-based nano coating material is prepared from a solid phase and a liquid phase according to a mass ratio of 1: 1, the solid phase consists of the following raw materials: 35 wt% of kaolin, 15 wt% of cobalt blue, 27 wt% of quartz powder, 12 wt% of iron oxide red, 5wt% of alumina short fiber and 6 wt% of filler; the liquid phase consists of 55 wt% of silica hybrid and 45 wt% of PAI, and the filler is titanium dioxide.
3. A preparation process of a microcrack diagnosis circuit based on a water-based nano coating is characterized by comprising the following steps: the aqueous nanocoating material of any one of claims 1 or 2, the process for preparing the microcrack diagnostic circuit comprising the steps of:
step 1, mixing the water-based nano coating materials according to the proportion, stirring for 5-10 hours at the rotating speed: 20-50 rpm; temperature: normal temperature;
step 2, spraying three layers of water-based nano coating materials on the workpiece;
step 3, carrying out laser direct graphical processing on the workpiece after the spraying is finished;
step 4, placing the workpiece treated in the step 3 into ultrasonic dust removal equipment for treatment for 5-15 minutes, wherein the water dripping time is 20-30 seconds, and the treatment is carried out in an environment of 50-60 ℃;
step 5, subjecting the workpiece subjected to ultrasonic treatment to two washing treatments at normal temperature, wherein the washing treatment lasts for 1-2 minutes, the dripping time lasts for 15-30 seconds, and air stirring is adopted in the washing treatment process;
step 6, carrying out copper impact treatment on the workpiece washed in the step 5 at the temperature of 50-62 ℃, wherein the treatment time is 10-30 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 7, carrying out two washing treatments on the workpiece treated in the step 6 at a normal temperature, wherein the washing treatment time is 0.5-1 minute, the dripping time is 20-30 seconds, and air stirring is adopted in the washing treatment process;
step 8, carrying out chemical thick copper plating treatment on the workpiece treated in the step 7 at the temperature of 50-56 ℃, wherein the treatment time is 60-180 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 9, carrying out three pure water washing treatments on the workpiece treated in the step 8 at normal temperature, wherein the water washing treatment time is 30 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the water washing treatment process;
step 10, performing pre-dipping treatment on the workpiece treated in the step 9 through a middle conversion hanger at normal temperature, wherein the treatment time is 3-5 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the pre-dipping treatment process;
step 11, performing nickel pre-activation treatment on the workpiece treated in the step 10 at the temperature of 32-38 ℃, wherein the treatment time is 5-10 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts mechanical circulation;
step 12, carrying out two times of pure water washing treatment on the workpiece treated in the step 11 at normal temperature, wherein the water washing treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the water washing treatment process;
step 13, carrying out post-dipping treatment on the workpiece treated in the step 12 in a normal temperature environment, wherein the treatment time is 2-5 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 14, carrying out three times of pure water washing treatment on the workpiece treated in the step 13 at normal temperature, wherein the treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the treatment process;
step 15, carrying out chemical nickel treatment on the workpiece treated in the step 14 at the temperature of 60-85 ℃, wherein the treatment time is 10-25 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts any one of air stirring or mechanical circulation;
step 16, performing two times of pure water washing treatment on the workpiece treated in the step 15 at normal temperature, wherein the treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the treatment process;
step 17, performing nickel-gold protection treatment on the workpiece treated in the step 16 at the temperature of 35-45 ℃, wherein the treatment time is 3-8 minutes, the water dripping time is 20-30 seconds, and the treatment process adopts mechanical circulation;
step 18, carrying out three times of pure water washing treatment on the workpiece treated in the step 17 at normal temperature, wherein the treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the treatment process;
and 19, carrying out hot water washing treatment on the workpiece treated in the step 18 at the temperature of 60-70 ℃, wherein the treatment time is 1-2 minutes, the water dripping time is 20-30 seconds, and air stirring is adopted in the treatment process.
4. The process for preparing the microcrack diagnosis circuit based on the water-based nano-coating according to claim 3, wherein the steps of: the three-layer aqueous nano-coating prepared in the step 2 of claim 3 has thickness distribution that: bottom layer: 6-12 microns; middle layer: 12-20 microns; surface layer: 15-20 microns.
5. The process for preparing the microcrack diagnosis circuit based on the water-based nano-coating according to claim 3, wherein the steps of: the laser processing parameters in the laser direct patterning method are filling distance <50 microns, scanning frequency 40-100 kilohertz, scanning speed 1000-2500 mm/s, power 7-10 watts, laser wavelength: 1064 nm.
6. The process for preparing the microcrack diagnosis circuit based on the water-based nano-coating according to claim 3, wherein the steps of: step 6 the impact copper treatment process uses a solution comprising the following components: 200 parts of copper complexing agent 150-; wherein, the copper complexing agent is EDTA and sodium potassium tartrate according to the weight ratio of 1: 1.
7. The process for preparing the microcrack diagnosis circuit based on the water-based nano-coating according to claim 6, wherein the steps of: the preparation method of the solution used in the impact copper treatment process in the step 6 comprises the following steps:
a) adding 350-500 parts of deionized water into a prepared clean plating bath;
b) starting air stirring, and adding 150 and 200 parts of copper complexing agent;
c) adding 20-40 parts of copper sulfate;
d) adding 1-5 parts of methanol;
e) adding 25-35 parts of sodium hydroxide;
f) then adding 350-500 parts of deionized water to the liquid preparation amount;
g) heating the plating tank to 54-62 ℃;
h) adding 12-18 parts of formaldehyde;
i) and (3) after the temperature is raised to the operating condition, analyzing the concentrations of the complexing agent, the copper ions, the formaldehyde and the sodium hydroxide, and adjusting the feeding in the process range for trial production.
8. The process for preparing the microcrack diagnosis circuit based on the water-based nano-coating according to claim 3, wherein the steps of: the solution used in the chemical thick copper plating treatment process in the step 8 comprises the following components: 180 portions of copper complexing agent 120, 20 to 25 portions of copper sulfate, 0.4 to 0.8 portion of methanol, 20 to 25 portions of sodium hydroxide, 8 to 12 portions of formaldehyde and 1000 portions of deionized water 700; wherein, the copper complexing agent is EDTA and sodium potassium tartrate according to the weight ratio of 1: 1.
9. The process for preparing the microcrack diagnostic circuit based on the water-based nanocoating according to claim 8, wherein:
the preparation method of the solution used in the chemical thick copper plating treatment process in the step 8 comprises the following steps:
a) adding 350-500 parts of deionized water into a prepared clean plating bath;
b) starting air stirring, and adding 120 and 180 parts of copper complexing agent;
c) adding 20-25 parts of copper sulfate;
d) adding 0.4-0.8 part of methanol;
e) adding 20-25 parts of sodium hydroxide;
f) then adding 350-500 parts of deionized water to the liquid preparation amount;
g) heating the plating tank to 50-56 ℃;
h) adding 8-12 parts of formaldehyde;
i) and (3) after the temperature is raised to the operating condition, analyzing the concentrations of the complexing agent, the copper ions, the formaldehyde and the sodium hydroxide, and adjusting the feeding in the process range for trial production.
10. Use of a process for the preparation of a microcrack diagnostic circuit based on aqueous nanocoatings according to any of claims 3 to 9, wherein said use is in the surface of bearings.
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