CN116273774A - Surface coating of semiconductor thermoelectric device and coating method - Google Patents
Surface coating of semiconductor thermoelectric device and coating method Download PDFInfo
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/60—Deposition of organic layers from vapour phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- 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 surface coating and a coating method of a semiconductor thermoelectric device, which belong to the technical field of semiconductor thermoelectric device processing, and the polymer of poly-p-xylene is deposited, and liquid phase separation does not occur, so that the poly-p-xylene does not suffer from any flow vacuum metal coating at the pressure of not more than 10 < -5 > Torr, and the adverse influence of the poly-p-body effect is caused by solvent, catalyst or plasticizer of the phenomena of gas outlet or gas outlet. Is non-line-of-sight deposition, the gaseous monomer acts uniformly on each side of the object to be coated, thereby forming a true pinhole-free conforma coating, and the parylene deposition process comprises three distinct steps. The first step is the vaporization of the solid dimer at around 150 ℃. The second step is to quantitatively cleave (pyrolyze) the dimer vapor at 680 ℃ to break two methylene bonds and obtain stable double free radical active monomer, and the monomer vapor enters a room temperature deposition chamber to polymerize on the substrate.
Description
Technical Field
The invention relates to the technical field of semiconductor thermoelectric device processing, in particular to a semiconductor thermoelectric device surface coating and a coating method.
Background
Thermoelectric devices have been widely used in industrial equipment such as laser diode temperature control, constant temperature bath, battery cabinets, etc. because of their excellent refrigerating effect. Also in recent years, with the rapid development of peltier technology and thermoelectric materials, thermoelectric elements and thermoelectric modules are also gradually applied to temperature control of household products such as dehumidifiers, ice cream machines, wine cabinets and seats.
Patent number CN202111192027.1 discloses a semiconductor thermoelectric device and a method for manufacturing the same, comprising a substrate, a plurality of thermoelectric particles and a circuit layer, wherein the substrate is made of heat-resistant insulating rigid heat-insulating material, and is provided with a plurality of through holes penetrating along the thickness direction; each thermoelectric particle is positioned in a corresponding through hole, each thermoelectric particle is directly formed by melting and solidifying powder of a material of the thermoelectric particle in each through hole, and each thermoelectric particle is respectively positioned at two opposite surfaces of the substrate along the thickness direction at two ends of the corresponding through hole; the two circuit layers are directly formed on opposite surfaces of the substrate in the thickness direction and electrically connect the plurality of thermoelectric particles, and each thermoelectric particle is completely enclosed in the corresponding through hole by the two circuit layers.
The patent solves the problem that as the semiconductor thermoelectric device enters the ultra-miniature stage, the physical cutting mode is not beneficial to miniaturization because of being limited to a cutting process; but cannot have optical characteristics and radiation resistance, has biocompatibility and biostability, and can be applied to various occasions.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a surface coating and a coating method of a semiconductor thermoelectric device.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the surface coating of the semiconductor thermoelectric device comprises silicon aluminum, toluene, dimethyl carbonate and dimethylbenzene.
Preferably, HZSM-5 with a silicon-aluminum ratio of 25 is used as a catalyst, toluene and dimethyl carbonate are used as raw materials, the molar ratio of the catalyst to the dimethyl carbonate is 3:1, the reaction temperature is 380 ℃, the conversion rate of toluene reaches 36.7%, and the selectivity to dimethyl benzene is 75.8%.
A method of coating a surface coating of a semiconductor thermoelectric device, comprising the steps of:
s1: the deposition process of the poly-p-xylene polymer is carried out, and the liquid phase separation does not occur, so that the poly-p-xylene does not suffer from any flow vacuum metal coating, and the pressure of the poly-p-xylene is not more than 10 < -5 > Torr, and the adverse effect of the poly-p-xylene is avoided;
s2: solvents, catalysts or plasticizers due to out-gassing or out-gassing. Non-line-of-sight deposition, the gaseous monomer uniformly acts on each surface of the object to be coated, thereby forming a true pinhole-free conformal coating;
s3: the parylene deposition process involves three distinct steps. The first step is the vaporization of the solid dimer at around 150 ℃. The second step is to quantitatively crack (pyrolyze) the dimer vapor at 680 ℃ to break two methylene bonds and obtain stable double free radical active monomer;
s4: the monomer vapor enters the room temperature deposition chamber and polymerizes on the substrate.
Preferably, in step S1, the fluid effect may cause concentration, flow, bridging, and xylene deposition is performed at a pressure of about 0.1 Torr.
Preferably, in the step S2, parylene is also free from leaching which may occur, and the average free space of gas molecules in the deposition chamber is Cheng Yaowei 0.1.1 cm.
Preferably, in the step S2, the substrate to be coated only needs to have a reasonable vacuum resistance.
Preferably, in the step S4, the substrate temperature is maintained at a room temperature level during the coating process.
Compared with the prior art, the invention has the beneficial effects that:
1. has high barrier property and chemical barrier property;
2. the heat-resistant and heat-resistant composite material has the characteristics of heat performance, low-temperature performance, vacuum stability and sterilization;
3. the high vacuum stability and the physical and mechanical properties of the poly-p-xylene sterilization are achieved;
4. the heat-resistant and heat-resistant composite material has the characteristics of heat performance, low-temperature performance, vacuum stability and sterilization;
5. has physical and mechanical properties;
6. the optical fiber has optical characteristics and radiation resistance, has biocompatibility and biostability, and can be applied to various occasions.
Drawings
Fig. 1 is a schematic flow chart of a method for coating a surface coating of a semiconductor thermoelectric device according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Referring to FIG. 1, example 1
The surface coating of the semiconductor thermoelectric device comprises silicon aluminum, toluene, dimethyl carbonate and dimethylbenzene.
HZSM-5 with the silicon-aluminum ratio of 25 is used as a catalyst, toluene and dimethyl carbonate are used as raw materials, the molar ratio of the catalyst to the dimethyl carbonate is 3:1, the reaction temperature is 380 ℃, the toluene conversion rate reaches 36.7%, and the selectivity to dimethylbenzene is 75.8%.
A method of coating a surface coating of a semiconductor thermoelectric device, comprising the steps of:
s1: the poly-p-xylene polymer is deposited, and since no liquid phase separation occurs, the poly-p-xylene is not subjected to any flow vacuum metallizing at a pressure of no more than 10 < 5 > Torr, while the poly-p-xylene effect is adversely affected, in step S1, the flow effect can cause concentration, flow, bridging, and the xylene deposition is performed at a pressure of about 0.1 Torr;
s2: solvents, catalysts or plasticizers due to out-gassing or out-gassing. Non-line-of-sight deposition, wherein gaseous monomers uniformly act on all sides of an object to be coated to form a real pinhole-free conformal coating, and in the step S2, parylene is not likely to be immersed, so that the average free space Cheng Yaowei 0.1.1 cm of gas molecules in a deposition chamber is avoided; in the step S2, the substrate to be coated only needs to have reasonable vacuum resistance;
s3: the parylene deposition process involves three distinct steps. The first step is the vaporization of the solid dimer at around 150 ℃. The second step is to quantitatively crack (pyrolyze) the dimer vapor at 680 ℃ to break two methylene bonds and obtain stable double free radical active monomer;
s4: the monomer vapor enters the room temperature deposition chamber and polymerizes on the substrate, and in step S4, the substrate temperature is maintained at room temperature level during the coating process.
Example 2
Thin film dielectric properties: the parylene coating is characterized by a very thin thickness, even a very thin parylene film, having excellent dielectric withstand voltage properties, and also shows that as the film thickness decreases, the breakdown voltage per unit thickness increases;
insulation resistance of circuit board: the key test for the protection provided by parylene coating is to coat the circuit board according to the test mode (as described in MIL-I-46058C) and measure the insulation resistance of the circuit board in one temperature and humidity cycle (MIL-STD-202, methods 106 and 302). Briefly, the test consisted of 10 cycles (daily-one cycle), each cycle containing seven steps. These seven steps cover a range of low temperature, low humidity (25 ℃, 50% relative humidity) conditions and more severe conditions (65 ℃, 90% relative humidity). In the test over a period of 10 days, resistance readings were taken at the beginning of each cycle and at 65℃and 90% relative humidity. Table 2 shows the results of testing parylene c.coating thicknesses of 50.8 microns to 2.5 microns. It is worth mentioning that even very thin coatings (2.5 microns) have insulation resistance values that are about an order of magnitude higher than the specified values.
Example 3
Has high barrier property and chemical barrier property
Barrier properties: the barrier properties of the parylene are shown in table 3. The water vapor transmission rates of parylene C and ParyFree are lower than most common polymeric materials, as compared to the Water Vapor Transmission Rates (WVTR) of other conforma coating materials;
chemical barrier: parylene is resistant to chemical attack and insoluble in all organic solvents at temperatures of 150 ℃. The expansion rate of the poly-p-xylene film after being exposed to various chemicals such as corrosive automobile and aviation fluids is very low; and after removal of the solvent by vacuum drying, the swelling was completely reversed (characterization of swelling by FTIR analysis). Other tests showed that the physical and chemical properties of the film were unchanged.
Example 4
Has thermal performance, low temperature performance, vacuum stability and sterilization characteristics
Thermal performance: arrhenius extrapolation, parylene N, paryFree and parylene C based on experimental data were expected to be continuously exposed to air at 60 ℃, 60 ℃ and 80 ℃ for up to 10 years, respectively. In an anaerobic or space vacuum environment, it is expected that parylene may be exposed to a temperature of 220 ℃ for as long as possible. Scs parylene HT has been demonstrated to be sustainable to exposure to air at 350 ℃, or to air at 450 ℃ for no more than 24 hours. In all cases, higher temperatures shorten the service life. If the requirements of the application are approaching or exceeding these time-temperature-atmospheric conditions, it is recommended to test the entire structure under conditions that more closely approximate the actual situation of the intended application.
Low temperature performance: at a low temperature of-200 ℃, the unsupported 50.8-micrometer thickness parylene C film fails after 6 times of 180 DEG bending. And films of polyethylene, polyethylene terephthalate and polytetrafluoroethylene fail after three, two and one bending respectively.
The steel sheet coated with parylene C and cooled in liquid nitrogen at-196℃withstands impacts above 11.3 N.m. in the modified Gardner ball drop impact test, which is about 28.2 N.m. at room temperature.
Supported parylene N films have proven to withstand thermal cycling from room temperature to-269 c low temperatures without cracking, spalling from the substrate, or electrical performance degradation.
Example 5
Has high vacuum stability
The weight loss of the poly-p-xylene N is 0.30 percent under the conditions that the temperature is 49.4 ℃ and the pressure is 10-6 Torr. Vacuum stability tests performed according to astm e595 at the golad space center of NASA showed that SCS parylene C and parylene ht were 0.07% and 0.03% weightless, respectively. The corresponding values for the volatile curable materials collected were 0.0003% and 0.0017%, respectively.
Example 6
Sterilization of parylene
Parylene N, C and parylene ht have been tested by a variety of sterilization methods including autoclaving, gamma and electron beam irradiation, hydrogen peroxide plasma and ethylene oxide. Post-sterilization analysis the effect of these sterilization methods on parylene N, C and parylene ht samples was evaluated by comparison with non-sterilized control samples. Evaluation of electrical, barrier and mechanical properties after sterilization showed that these properties did not change in most of the tests performed on these parylene variants.
Example 7
The physical and mechanical properties are: since parylene has a large molecular weight (about 500,000), a high melting temperature, and a high crystallinity, it cannot be molded by conventional methods such as extrusion or compression molding. At temperatures not higher than 175 ℃, their solubility in organic or other media is very low and therefore cannot be shaped by casting;
the parylene polymer was excellent in impact resistance when supported by the test plate. The results of the "Q" steel test panels coated with 25.4 microns thick parylene C in the Gardner ball drop impact test were around 28.2 N.m;
the abrasion resistance index was measured to be 22.5 for parylene C and 8.8 for parylene N. In contrast, polytetrafluoroethylene was 8.4, high impact polyvinyl chloride was 24.4, epoxy resin was 41.9, and polyurethane was 59.5;
the annealing treatment can enhance the cut-through resistance, increase the hardness and improve the wear resistance of the parylene. This is a result of the increased polymer density and crystallinity.
Example 8
Has optical properties and radiation resistance
Optical properties: parylene absorbs little in the visible range and is therefore transparent and colorless. At wavelengths less than 280 nm, all parylene is strongly absorbed.
Radiation resistance: under the action of gamma rays in vacuum, the parylene N, C, D and ParyleHT films show high resistance to degradation. The tensile and electrical properties remain unchanged after exposure to a radiation dose of 1,000 kgy at a radiation dose rate of 16 kgy/hr. Exposure to air can lead to rapid embrittlement;
although parylene N, C, D and ParyFree are stable in indoor performance, it is not recommended to use them in direct sunlight (uv) environments for a long period of time. Paryleht has remarkable ultraviolet resistance, and no performance degradation occurs after exposure to air for up to 2,000 hours of ultraviolet accelerated aging test.
Example 9
The SCS parylene N, C and ParyleHT were tested for biocompatibility and biostability according to the biological evaluation requirements of ISO 10993. Furthermore, the biocompatibility and biostability of SCS parylene has been verified in a variety of medical coating applications over the last 40 years.
Example 10
The conforma coating is widely applied to industries such as electronics, medical instruments, transportation, aerospace, national defense and the like, and provides protection, biostability and surface modification for application occasions so as to enhance the overall reliability of components and final products. Factors affecting adhesion, such as surface contamination, presence of oxide layers and low surface energy substrates, can adversely affect reliability;
treatment with a-174 silane coupling agent prior to the application of the parylene generally results in desirable adhesion of the parylene to a variety of substrates. However, there are times when very high standards cannot be met on many highly difficult substrates (such as high polished stainless steel, titanium, dissimilar alloys, and polyimide, etc.). The SCSAdPro series technique enhances adhesion between parylene coatings and substrates that are challenging.
They have proven to be stable at high temperatures, making them excellent adhesion enhancing tools suitable for harsh environment applications. Customers using SCS business coating services may share AdPro adhesion enhancement technology.
Example 11
Application of the method is as follows:
1. electronic product
The SCS parylene coating is uniformly shaped to ensure complete encapsulation of the circuit board, core and other electronics packages, such as microelectromechanical systems, lab-on-a-chip technology and sensors. SCS parylene C coatings have been shown to inhibit whisker, abnormal protrusion (OSE) and dendrite formation;
2. medical treatment
SCs parylene has gained FDA approval and provides ideal surface modification for catheters, seals, stents, cochlear implants, surgical tools, cardiac pacemakers, and components, etc., implanted and non-implanted medical devices. The parylene coating helps the devices and components resist attack by moisture, biological fluids and biological gases, and acts as a biocompatible surface in contact with biological tissue;
3. transportation and transportation
Ultra-thin parylene coatings provide protection for important sensors, circuit boards and other components in home automobiles and heavy duty engines and systems, and are resistant to attack by corrosive chemicals, fluids and gases even at high temperatures and long periods of use;
4. aerospace and national defense
SCS parylene provides excellent protection for a number of applications in the aerospace and defense industries including aircraft, space planning and defense systems. The parylene coating can reliably resist the effects of moisture, dust, sand, chemical and biological agents and the like;
in the invention, the installation mode, the connection mode or the setting mode of all the components are common mechanical modes, and the specific structure, the model and the coefficient index of all the components are self-contained technologies, so long as the beneficial effects can be achieved, the implementation can be carried out, and redundant description is omitted.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
In the present invention, unless otherwise indicated, the terms "about" and "front and back," inner and outer, and vertical levels, "etc., used herein are merely intended to refer to the orientation of the term in conventional use, or are colloquially known to those skilled in the art, and should not be construed as limiting the term, while the terms" first, "second," and "third," etc., do not denote a particular number or order, but are merely intended to be used in distinguishing between the terms, and the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements, but also include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Claims (7)
1. The surface coating of the semiconductor thermoelectric device is characterized by comprising silicon aluminum, toluene, dimethyl carbonate and dimethylbenzene.
2. The surface coating of the semiconductor thermoelectric device according to claim 1, wherein HZSM-5 with a silicon-aluminum ratio of 25 is used as a catalyst, toluene and dimethyl carbonate are used as raw materials, the molar ratio of toluene and dimethyl carbonate is 3:1, the reaction temperature is 380 ℃, the conversion rate of toluene reaches 36.7%, and the selectivity to dimethyl benzene is 75.8%.
3. A method of coating a surface coating of a semiconductor thermoelectric device, comprising the steps of:
s1: the deposition process of the poly-p-xylene polymer is carried out, and the liquid phase separation does not occur, so that the poly-p-xylene does not suffer from any flow vacuum metal coating, and the pressure of the poly-p-xylene is not more than 10 < -5 > Torr, and the adverse effect of the poly-p-xylene is avoided;
s2: solvents, catalysts or plasticizers due to out-gassing or out-gassing. Non-line-of-sight deposition, the gaseous monomer uniformly acts on each surface of the object to be coated, thereby forming a true pinhole-free conformal coating;
s3: the parylene deposition process involves three distinct steps. The first step is the vaporization of the solid dimer at around 150 ℃. The second step is to quantitatively crack (pyrolyze) the dimer vapor at 680 ℃ to break two methylene bonds and obtain stable double free radical active monomer;
s4: the monomer vapor enters the room temperature deposition chamber and polymerizes on the substrate.
4. A method of coating a surface of a semiconductor thermoelectric device according to claim 3, wherein in step S1, the fluid effect causes concentration, flow, bridging, and the xylene deposition is performed at a pressure of about 0.1 torr.
5. A method of coating a surface of a semiconductor thermoelectric device according to claim 3, wherein in step S2, parylene is also free of possible leaching, and the average free of gas molecules in the deposition chamber is Cheng Yaowei 0.1.1 cm.
6. A method of coating a surface coating of a semiconductor thermoelectric device according to claim 3, wherein in step S2, the substrate to be coated is only required to have a reasonable vacuum resistance.
7. A method of coating a surface coating of a semiconductor thermoelectric device according to claim 3, wherein in step S4, the substrate temperature is maintained at a room temperature level during the coating process.
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| CN115710836A (en) * | 2022-10-24 | 2023-02-24 | 国网浙江省电力有限公司电力科学研究院 | Method for improving insulation aging resistance of vegetable oil paper |
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| CN115710836A (en) * | 2022-10-24 | 2023-02-24 | 国网浙江省电力有限公司电力科学研究院 | Method for improving insulation aging resistance of vegetable oil paper |
| CN115710836B (en) * | 2022-10-24 | 2023-12-12 | 国网浙江省电力有限公司电力科学研究院 | Method for improving insulation ageing resistance of vegetable oil paper |
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