CN113584432B - Preparation technology of non-vacuum high-temperature solar selective absorbing coating - Google Patents

Preparation technology of non-vacuum high-temperature solar selective absorbing coating Download PDF

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CN113584432B
CN113584432B CN202110899043.8A CN202110899043A CN113584432B CN 113584432 B CN113584432 B CN 113584432B CN 202110899043 A CN202110899043 A CN 202110899043A CN 113584432 B CN113584432 B CN 113584432B
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power supply
solar selective
deposition
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CN113584432A (en
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宫殿清
杨鹏
李克伟
崔泽琴
王晓波
韩彦莎
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Taiyuan University of Technology
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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Abstract

The invention discloses a preparation technology of a non-vacuum high-temperature solar selective absorption coating. This technique is used for the preparation of non-vacuum high temperature solar selective absorbing coatings. Based on the existing mature solar selective absorbing coating, the Cu infrared reflecting layer and the isolating layer are prepared by using a multi-arc ion plating process, so that the coating can work for a long time in a non-vacuum environment with the temperature of more than 500 ℃. The invention requires strict control of chamber air pressure, air purity and proportion, target size and purity, deposition current density, bias voltage and deposition time in the processing process, so that the diffusion distance of each layer in the preparation process is less than 10 nm, and the components in the processing process are kept stable. The invention has the characteristics of high deposition efficiency, strong adaptability to the base material, high product quality stability, low energy consumption and low cost.

Description

Preparation technology of non-vacuum high-temperature solar selective absorbing coating
Technical Field
The invention relates to the field of solar heat utilization, in particular to a preparation technology of a non-vacuum high-temperature solar selective absorption coating.
Background
With the continuous consumption of various non-renewable resources on the earth, the problem of resource shortage is also becoming a concern, and the use of renewable energy sources is also becoming an important issue at present. Solar energy is the most important energy source in renewable energy sources, and has great research value. Solar collectors are key devices for converting solar energy into thermal energy, and their photo-thermal conversion efficiency has a decisive influence on reducing the cost of solar heat utilization. And the solar selective absorption coating with excellent performance can improve the photo-thermal conversion efficiency of the solar heat collector by 8-10 times, so that the solar heat collector has been paid attention to widely. Currently, such coatings can be prepared by a variety of means, but most fail under non-vacuum high temperature conditions due to diffusion of low melting components and oxidation of the substrate. In order to popularize the use of the material and reduce the cost of high-temperature solar energy application such as solar thermal power stations, it is necessary to develop a preparation technology of a solar selective absorption coating capable of preventing diffusion of low-melting components and oxidation of a substrate.
Disclosure of Invention
The invention provides a preparation technology of a non-vacuum high-temperature solar selective absorbing coating, which aims to solve the technical problem that the existing solar selective absorbing coating fails due to low-melting component diffusion and matrix oxidation at a non-vacuum high temperature.
The invention is realized by adopting the following technical scheme: a preparation technology of a non-vacuum high-temperature solar selective absorbing coating adopts a multi-arc ion plating technology to deposit Cu on a workpiece as an infrared reflecting layer, an isolating layer is deposited on the infrared reflecting layer, and a solar selective absorbing coating is deposited on the isolating layer.
The invention deposits the isolation layer on the infrared reflecting layer, the isolation layer can effectively prevent the diffusion of low-melting components and the oxidation function of the matrix, so that the invention can keep good absorptivity and emissivity for a long time (more than 3 months) under the environment of non-vacuum high temperature (more than 500 ℃). Theoretically, the infrared reflecting layer with the best optical performance is a Cu metal layer at present. However, the Cu metal layer diffuses in an environment of 300 ℃ or higher. The diffused Cu element intrudes into the absorption layer, resulting in a change in the composition of the absorption layer, so that the optical properties of the coating layer are deteriorated. According to the invention, through designing the isolation layer, cu diffusion can be effectively prevented, components and performances of each part of the coating are maintained stable, and the use temperature of the coating is improved. Considering the requirement of the solar selective absorption coating, the isolation layer is required to have good high-temperature stability (namely no phase change at high temperature and no change of chemical components), is tightly combined with the infrared reflection layer and the absorption layer, and has small influence on the reflectivity of the coating (the ratio of the absorption rate to the emissivity is more than 6).
Further, the invention is realized by the following steps:
(1) Installing a Cu target and an isolating layer target, installing the matched Cu target and the isolating layer target in a multi-arc ion plating furnace, and installing the Cu target and the isolating layer target relatively;
(2) Cleaning a workpiece; firstly removing rust and a protective film on the surface of a workpiece by mechanical means, then flushing with purified water for about 3 minutes, then immersing in acetone or absolute ethyl alcohol, and cleaning for about 20 minutes by an ultrasonic vibration mode; taking out and drying after cleaning;
(3) Installing a workpiece, namely installing the workpiece on a sample table in the multi-arc ion plating furnace, wherein the surface to be plated is opposite to the Cu target; measuring the distance between the workpiece and the target;
(4) Vacuum pumping to lock the furnace door, opening the vacuum system to pump vacuum, and maintaining the air pressure in the furnace at 1×10 -2 ±0.005Pa；
(5) Introducing working gas, wherein the working gas is Ar gas, and the air pressure is maintained to be 0.5+/-0.05 Pa;
(6) Cleaning the Cu target, setting the bias voltage to 800V, turning on the bias power supply and the arc power supply, cleaning the Cu target for 2+/-0.05 minutes, and then turning off the bias power supply and the arc power supply;
(7) Setting a deposition current and a bias deposition currentIAccording to the area of the target materialA) The current is determined to be ampere (A) and the area is determined to be square centimeter (cm) 2 ) Bias voltage magnitudeU bias According to the distance between the target and the sampleLDetermining that the bias voltage is in volts (V), the distance is in centimeters (cm), and no more than 400V; the calculation formula is as follows:
𝐼=0.4∙𝐴
𝑈 𝑏𝑖𝑎𝑠 =10∙𝐿；
(8) Setting the Cu plating time to be 2+/-0.05 minutes;
(9) Firstly, starting a bias power supply and then starting an arc power supply when deposition is started, and if the equipment is provided with an observation window, paying attention to whether an arc is stable or not in the deposition process;
(10) Ending the deposition 2+/-0.05 minutes later, closing an arc power supply and a bias power supply, and keeping Ar gas to be introduced into the furnace;
(11) Setting the bias voltage of the target material for cleaning the isolation layer to 800V, switching on the bias voltage power supply and the arc power supply, cleaning the target material for cleaning the isolation layer for 2+/-0.05 minutes, and switching off the bias voltage power supply and the arc power supply;
(12) Adjusting the components of the working gas to Ar gas and N 2 Mixed gas of gases, N 2 The flow rate of the gas is 80sccm, and Ar gas is regulated according to the pressure in the furnace, so that the pressure in the furnace is maintained to be 0.5+/-0.05 Pa;
(13) The set deposition current and bias deposition current calculation formulas are as follows:
𝐼=0.5∙𝐴
𝑈 𝑏𝑖𝑎𝑠 =10∙𝐿 ；
(14) Setting the time to be 1+/-0.05 minutes when the isolation layer is plated at the set time;
(15) Rotating the sample stage to enable the workpiece to be plated to face the isolating layer target;
(16) Firstly, starting a bias power supply and then starting an arc power supply when deposition is started, and if the equipment is provided with an observation window, paying attention to whether an arc is stable or not in the deposition process;
(17) Ending the deposition to turn off the arc power supply and the bias power supply;
(18) Stopping the working gas from being introduced;
(19) Stopping vacuumizing;
(20) The air inlet valve is opened by air inlet, and the air pressure inside and outside the furnace is finally consistent;
(21) Taking out the product;
(22) Disassembling all targets;
(23) And preparing the solar selective absorption coating.
The invention requires strict control of chamber air pressure, air purity and proportion, target size and purity, deposition current density, bias voltage and deposition time in the processing process, so that the diffusion distance of each layer in the preparation process is less than 10 nm, and the components in the processing process are kept stable. The solar selective absorption coating provided by the invention has the advantages that the high-temperature stability and the isolation effect of the solar selective absorption coating are considered, and the optical performance of the solar selective absorption coating is also considered, so that the preparation process parameters are the most critical, and the innovation of the solar selective absorption coating is also realized. If the process parameters are incorrect, in particular the deposition time, deposition current, bias voltage are incorrect, an effective coating cannot be obtained; only by adopting the process parameters and steps, the effective coating with high-temperature stability and good isolation effect and optical performance meeting the requirements can be obtained. The invention has the characteristics of high deposition efficiency, strong adaptability to the base material, high product quality stability, low energy consumption and low cost, has good functions of preventing the diffusion of low-melting components and the oxidation of the base body, and ensures that the coating can be normally used in a non-vacuum high-temperature environment.
Drawings
FIG. 1 shows the results of a high temperature test without barrier coating. Experimental conditions: the temperature is kept for 100 hours at 600 ℃ in the atmospheric environment.
Before the test: absorption rate 0.827, emissivity 0.103; after testing: absorption rate 0.759 and emissivity 0.138.
FIG. 2 shows the results of a high temperature test of barrier coating. The experimental conditions were the same as above.
Before the test: absorption 0.876, emissivity 0.125, after testing: absorption rate 0.910, emissivity 0.131.
As can be seen by comparing FIGS. 1 and 2, the isolation coating prepared by the process of the invention has small change of the absorptivity and emissivity of the whole solar absorbing coating before and after a high temperature test, and can meet the use requirement in a non-vacuum high temperature environment.
FIG. 3 comparison of Cu diffusion before high temperature testing (left panel) and after high temperature testing (right panel); the horizontal axis is the distance from the surface of the coating.
FIG. 4 is a comparison of Cu diffusion before (left) and after (right) high temperature testing of barrier coatings; the horizontal axis is the distance from the surface of the coating.
Figures 3 and 4 were obtained using EDS line scanning. Comparing fig. 3 and 4, it can be seen that the Cu diffusion range is very small at high temperature with the barrier coating, which is much smaller than without the barrier coating.
FIG. 5 shows the reflectance profile of a solar selective absorber coating prepared in accordance with the present invention before and after high temperature treatment. It can be seen that the coating prepared by the invention has very small variation amplitude of reflectivity after being treated by multiple high temperature conditions, and has little difference before being treated.
Fig. 6 is a schematic view of the structure of the solar selective absorbing coating according to the present invention.
Detailed Description
In the concrete implementation, the workpiece cannot use ferromagnetic materials or high polymer materials; non-ferromagnetic metal materials and ceramic materials are used, and the surface roughness of the surface to be plated cannot be higher than Ra 0.8 in Chinese standards.
The isolating layer is made of nitride of CrN, tiN or high-entropy alloy; the target material is Cr target, ti target or designed high-entropy alloy target. Such materials help to prevent diffusion of low melting components and matrix oxidation in the absorber coating.
The absorbing layer is all solar selective absorbing coatings which can be prepared by the current magnetron sputtering, radio frequency sputtering, multi-arc ion plating and other processes, and comprises but is not limited to AlN/AlNO/AlO, alCrN/AlCrNO/AlCrO and CrN/CrNO/CrO.
The deposition current density is determined according to the type and the size of the target material, and the precision is controlled to be +/-0.05A/cm 2 . The high-precision current is beneficial to the formation of the infrared reflecting layer and the isolation layer.
The purity of the gas used in each step is higher than 99.9%.
When a Cu layer and an isolation layer are deposited, a workpiece in the furnace is not contacted with the atmosphere; after depositing the Cu layer, the position of the workpiece is adjusted by rotating the sample table, and meanwhile, the oxidizing gas such as oxygen and the like is prevented from being introduced into the furnace by maintaining the working gas.
For a better understanding of the present invention, the present invention will be further described with reference to a specific example 1. The technical solutions claimed in the present invention are not limited to the following examples only.
Example 1
The present embodiment provides a multi-arcA method for preparing a high-temperature solar selective absorption coating containing a Cu reflecting layer and an isolating layer structure by ion plating. The workpiece is 304 stainless steel, the isolating layer is CrN, and the absorbing layer is AlCrN/AlCrNO/Al 2 O 3 Solar energy selective absorbing coating.
The preparation method of the solar selective absorbing coating comprises the following steps:
(1) And (5) installing a target. And relatively installing a Cu target and a Cr target matched with the multi-arc ion plating equipment at the target position in the multi-arc ion plating furnace. The areas of the targets are all 100cm 2 。
(2) And cleaning the workpiece. And wiping the surface of the workpiece by using soft cleaning cloth to remove the surface protection film and dust. Then rinsed with purified water for about 3 minutes. And then the surface to be plated is completely immersed into absolute ethyl alcohol. The washing was performed by ultrasonic vibration for about 20 minutes. And taking out immediately after cleaning, and rapidly drying at low temperature.
(3) And installing a workpiece. And installing the workpiece on the sample stage in the multi-arc ion plating. The surface to be plated faces the Cu target. And measuring the distance between the surface to be plated of the workpiece and the target. Take 20cm as an example.
(4) And (5) vacuumizing. And locking the furnace door. Opening a vacuum system to vacuumize, and maintaining the air pressure in the furnace at 1×10 -2 About Pa.
(5) Ar gas was introduced. The purity of Ar gas should be higher than 99.9%, and the gas pressure is maintained at 0.5.+ -. 0.05. 0.05 Pa.
(6) And cleaning the Cu target. The bias voltage was set to 800V, and the bias power and arc power were turned on to clean the Cu target for about 2 minutes. The bias power supply and the arc power supply are turned off.
(7) The deposition current and bias voltage are set. The deposition current and bias voltage magnitudes are calculated according to the formula. The deposition current in this example was 40A and the bias was 200V. The calculation process is as follows:
𝐼=0.4∙𝐴=0.4×100=40 (A) 𝑈 𝑏𝑖𝑎𝑠 =10∙𝐿=10×20=200 (V)
(8) Setting time. The set time for Cu plating was 2 minutes.
(9) Deposition is started. The bias power is turned on first and then the arc power is turned on. After 2 minutes the deposition was ended.
(10) And ending the deposition. The arc power and bias power are turned off. Ar gas is still kept to be introduced into the furnace.
(11) And cleaning the Cr target. The bias voltage was set to 800V, and the bias power and arc power were turned on to clean the Cr target for about 2 minutes. The bias power supply and the arc power supply are turned off.
(12) The composition of the working gas is adjusted. The working gas is Ar gas and N 2 A mixed gas of gases. Setting N 2 The flow rate of the gas was 80 sccm. Ar gas is regulated according to the pressure in the furnace, so that the pressure in the furnace is maintained to be 0.5+/-0.05 Pa.
(13) The deposition current and bias voltage are set. The deposition current in this example was 50A and the bias was 200V. The calculation process is as follows:
𝐼=0.5∙𝐴=0.5×100=50 (A) 𝑈 𝑏𝑖𝑎𝑠 =10∙𝐿=10×20=200 (V)
(14) Setting time. The time for plating CrN was set to 1 minute.
(15) And rotating the sample table to enable the workpiece to be plated to face the Cr target.
(16) Deposition is started. The bias power is turned on first and then the arc power is turned on. Deposit for 1 minute.
(17) And ending the deposition. The deposition was terminated after 1 minute, and the arc power and bias power were turned off.
(18) And stopping the working gas from being introduced.
(19) And stopping vacuumizing.
(20) Air is introduced. And opening an air inlet valve, and introducing air to finally make the air pressure inside and outside the furnace consistent.
(21) And taking out the workpiece.
(22) And disassembling the Cu target and the Cr target.
(23) And (5) installing an AlCr target.
(24) And cleaning the workpiece. The work piece was rinsed with purified water for about 3 minutes, then immersed in acetone or absolute ethanol, and rinsed by ultrasonic vibration for about 20 minutes. And taking out and drying after cleaning.
(25) And installing a workpiece. And installing the workpiece on a sample stage in the multi-arc ion plating furnace. The surface to be plated is required to face against the AlCr target.
(26) AlCrN/AlCrNO/Al plating 2 O 3 A layer.
(27) And taking out the workpiece.
In conclusion, cu/CrN/AlCrN/AlCrNO/Al prepared by utilizing multi-arc ion plating technology 2 O 3 The solar selective absorption coating has an absorptivity of 0.876 and an emissivity of 0.125. After annealing at 600 ℃ in air for 100 hours, the absorptivity is 0.910 and the emissivity is 0.131.

Claims (8)

1. A preparation technology of a non-vacuum high-temperature solar selective absorbing coating is characterized in that: cu is deposited on a workpiece by adopting a multi-arc ion plating technology to serve as an infrared reflecting layer, an isolating layer is deposited on the infrared reflecting layer, and a solar selective absorbing coating is deposited on the isolating layer; the isolating layer adopts nitride of CrN, tiN or high-entropy alloy; the method is realized by the following steps:
(1) Installing a Cu target and an isolating layer target, installing the matched Cu target and the isolating layer target in a multi-arc ion plating furnace, and installing the Cu target and the isolating layer target relatively;
(2) Cleaning a workpiece;
(3) Installing a workpiece, namely installing the workpiece on a sample table in the multi-arc ion plating furnace, wherein the surface to be plated is opposite to the Cu target;
(4) Vacuum pumping to lock the furnace door, opening the vacuum system to pump vacuum, and maintaining the air pressure in the furnace at 1×10 -2 ±0.005Pa；
(5) Introducing working gas, wherein the working gas is Ar gas, and the air pressure is maintained at 0.5+/-0.05 Pa;
(6) Cleaning the Cu target, setting the bias voltage to 800V, switching on the bias voltage power supply and the arc power supply, cleaning the Cu target for 2+/-0.05 minutes, and then switching off the bias voltage power supply and the arc power supply;
(7) Setting a deposition current and a bias deposition current I according to the target area A, wherein the current unit is ampere, the area unit is square centimeter, and the bias voltage is U bias According to the distance L between the target and the sample, the bias voltage unit is volt, the distance unit is cm, and the voltage is not more than 400V; the calculation formula is as follows:
I＝0.4·A
U bias ＝10·L；
(8) Setting the Cu plating time to be 2+/-0.05 minutes;
(9) Firstly, starting a bias power supply and then starting an arc power supply when deposition is started, and paying attention to whether an arc is stable or not in the deposition process;
(10) Ending the deposition 2+/-0.05 minutes later, closing an arc power supply and a bias power supply, and keeping Ar gas to be introduced into the furnace;
(11) Setting the bias voltage of the target material for cleaning the isolation layer to 800V, switching on the bias voltage power supply and the arc power supply, cleaning the target material for cleaning the isolation layer for 2+/-0.05 minutes, and switching off the bias voltage power supply and the arc power supply;
(12) Adjusting the components of the working gas to Ar gas and N 2 Mixed gas of gases, N 2 The flow rate of the gas is 80sccm, and Ar gas is regulated according to the pressure in the furnace, so that the pressure in the furnace is maintained at 0.5+/-0.05 Pa;
(13) The set deposition current and bias deposition current calculation formulas are as follows:
I＝0.5·A
U bias ＝10·L；
(14) Setting the time to be 1+/-0.05 minutes when the isolation layer is plated at the set time;
(15) Rotating the sample stage to enable the workpiece to be plated to face the isolating layer target;
(16) Firstly, starting a bias power supply and then starting an arc power supply when deposition is started, and paying attention to whether an arc is stable or not in the deposition process;
(17) Ending the deposition to turn off the arc power supply and the bias power supply;
(18) Stopping the working gas from being introduced;
(19) Stopping vacuumizing;
(20) The air inlet valve is opened by air inlet, and the air pressure inside and outside the furnace is finally consistent;
(21) Taking out the product;
(22) Disassembling all targets;
(23) And preparing the solar selective absorption coating.
2. The process for preparing a non-vacuum high-temperature solar selective absorption coating according to claim 1, wherein the workpiece cannot use ferromagnetic materials or polymeric materials; non-ferromagnetic metal materials and ceramic materials are used, and the surface roughness of the surface to be plated cannot be higher than Ra 0.8 in Chinese standards.
3. The preparation technology of the non-vacuum high-temperature solar selective absorbing coating according to claim 1, wherein the target material used for the isolating layer is a Cr target, a Ti target or a designed high-entropy alloy target.
4. The process for preparing a non-vacuum high-temperature solar selective absorbing coating according to claim 1, wherein the solar selective absorbing coating is all solar selective absorbing coatings prepared by the current magnetron sputtering, radio frequency sputtering and multi-arc ion plating processes, including but not limited to AlN/AlNO/AlO, alCrN/AlCrNO/AlCrO and CrN/CrNO/CrO.
5. The preparation technology of the non-vacuum high-temperature solar selective absorbing coating as claimed in claim 1, wherein the deposition current density is determined according to the type and the size of the target material, and the accuracy is controlled to be +/-0.05A/cm 2 。
6. The process for preparing a non-vacuum high temperature solar selective absorption coating according to claim 1, wherein the purity of the gas used in each step is higher than 99.9%.
7. The process for preparing a non-vacuum high-temperature solar selective absorption coating according to claim 1, wherein the workpiece in the furnace is not in contact with the atmosphere when depositing the Cu layer and the isolation layer; after depositing the Cu layer, the position of the workpiece is adjusted by rotating the sample table, and meanwhile, the oxidizing gas such as oxygen and the like is prevented from being introduced into the furnace by maintaining the working gas.
8. A process for preparing a non-vacuum high-temperature solar selective absorption coating according to claim 1, wherein,the area of the target material is 100cm 2 The distance between the surface to be plated of the workpiece and the target is 20cm; the deposition current in the step (7) is 40A, and the bias voltage is 200V; the deposition current in step (13) was 50A and the bias voltage was 200V.
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