CN114855142B - Low surface energy parylene material and its preparation method - Google Patents
Low surface energy parylene material and its preparation method Download PDFInfo
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- CN114855142B CN114855142B CN202210401691.0A CN202210401691A CN114855142B CN 114855142 B CN114855142 B CN 114855142B CN 202210401691 A CN202210401691 A CN 202210401691A CN 114855142 B CN114855142 B CN 114855142B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
Abstract
The invention provides a low-surface-energy parylene material and a preparation method thereof, which are based on the existing parylene material, the surface energy of the parylene material is reduced while the original excellent physical and chemical properties of the parylene material are maintained, and the surface of the parylene material after coating can reach a super-hydrophobic state by combining a substrate with a micro-nano structure, so that the self-cleaning property under certain specific working conditions is realized. The low surface energy parylene material is formed by chemical vapor deposition of a parylene raw material and a fluorine-containing reagent. The preparation method comprises the following steps: step 1, placing a parylene raw material and a fluorine-containing reagent into an evaporation chamber; step 2, vacuumizing the whole reaction device to ensure that the reaction occurs under the vacuum condition; step 3, firstly raising the temperature of the cracking furnace to 690 ℃ or 650 ℃, and then raising the temperature of the evaporating chamber to 175 ℃; and 4, depositing a film on the substrate in the room temperature chamber after the raw materials react.
Description
Technical Field
The invention relates to the technical field of functional material surfaces, in particular to a low-surface-energy parylene material and a preparation method thereof.
Background
Parylene (Parylene) is a novel dressing coating material developed and applied by Unioncarbide Co in the middle of sixties, is a polymer of paraxylene, and can be divided into N type, C type, D type, F type, HT type and the like according to different molecular structures. The parylene is a protective polymer material, chinese name, parylene and parylene can be vapor deposited under vacuum, and the good penetrability of parylene active molecules can form a transparent insulating coating with no pinholes and uniform thickness inside and at the periphery of the electronic element, so that a complete high-quality protective coating is provided for the element, and the infringement of acid, alkali, salt fog, mould and various corrosive gas parts is resisted.
However, the existing parylene material has the defects of higher surface energy, limited application scene and the like.
Disclosure of Invention
The invention provides a low-surface-energy parylene material and a preparation method thereof, which are based on the existing parylene material, the surface energy of the parylene material is reduced while the original excellent physical and chemical properties of the parylene material are maintained, and the surface of a coated film is enabled to reach a super-hydrophobic state by combining a substrate with a micro-nano structure, so that the self-cleaning property under certain specific working conditions is realized.
The technical problems to be solved by the invention are realized by the following technical scheme:
the invention provides a low-surface-energy parylene material, which is formed by chemical vapor deposition of a parylene raw material and a fluorine-containing reagent.
Preferably, the method comprises the steps of, the fluorine-containing reagent comprises 2,3, 4,5, 6, 7-dodecafluoro-1, 8-octanediol, 3-trifluoro ethyl propionate nine-carbon perfluoro polyether siloxane, 2-trifluoro ethyl ester perfluoropolyether, 2-trifluoroacetamide, perfluorononane, perfluorodecyl ethyl acrylate, undec fluoro-n-hexane-1-ol, perfluorodecane.
Preferably, the difference between the evaporation temperature of the parylene feedstock and the evaporation temperature of the fluorine-containing reagent is less than or equal to 25 ℃.
Preferably, the difference between the evaporation temperature of the parylene raw material and the evaporation temperature of the fluorine-containing reagent is 0 ℃ to 25 ℃.
Preferably, the cleavage temperature of the fluorine-containing reagent is less than 700 ℃.
A method for preparing a low surface energy parylene material, comprising the following steps:
step 1, placing a parylene raw material and a fluorine-containing reagent into an evaporation chamber;
step 2, vacuumizing the whole reaction device to ensure that the reaction occurs under the vacuum condition;
step 3, firstly raising the temperature of the cracking furnace to 690 ℃ or 650 ℃, and then raising the temperature of the evaporating chamber to 175 ℃;
and 4, depositing a film on the substrate in the room temperature chamber after the raw materials react.
Preferably, in said step 1, if the evaporation temperatures of the parylene feedstock and the fluorine-containing reagent differ by >10 ℃, the parylene feedstock and the fluorine-containing reagent should be placed separately into the evaporation chamber; if the evaporation temperatures of the parylene feedstock and the fluorogenic agent differ by <10 ℃, the parylene feedstock and the fluorogenic agent may be mixed and placed into the evaporation chamber.
Preferably, the substrate may be any material.
Preferably, if the base material is a metal substrate, a treatment for enhancing adhesion performance is required.
Preferably, the raw materials which cannot be deposited in the step 4 are adhered to the cold well rod at a low temperature through the cold well, and prevented from entering the vacuum pump.
The invention has the beneficial effects that:
1. the low-surface-energy parylene material has higher contact angle and excellent physicochemical properties, such as higher dielectric constant and better mechanical property;
2. the low-surface-energy parylene material has durability and stable performance based on the body property;
3. the parylene material with low surface energy has various adjustable factors and can flexibly adapt to the requirements of different application scenes;
4. the preparation method of the low-surface-energy parylene material is simple, the range of selectable raw materials is wide, the cost is low, and the mass production is facilitated.
Drawings
FIG. 1 is a schematic illustration of a method of preparing a low surface energy parylene material of the present invention;
FIG. 2 is a cross-section of a low surface energy parylene material of example 5 of the present invention with a porous structure;
FIG. 3 is a graph showing the results of contact angle test experiments for samples of low surface energy parylene materials of the present invention;
fig. 4 is the results of mechanical property testing experiments for samples of low surface energy parylene materials of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Fig. 1 is a schematic diagram of a method for preparing a low surface energy parylene material of the present invention. The low surface energy parylene material of the present invention can be prepared by the following method, and the specific method can be adjusted according to different factors of the parylene material and the fluorine-containing reagent. Specific methods are given below taking parylene C as a base material. The preparation of other base materials can be carried out by reference.
The preparation method comprises the following steps: CVD chemical vapor deposition
Step 1: placing the parylene C raw material and the fluorine-containing reagent into an evaporation chamber;
step 2: vacuumizing the whole reaction device to ensure that the reaction occurs under the vacuum condition;
step 3: the temperature of the cracking furnace was first raised to 690 c and then the temperature of the vaporization chamber was raised to 175 c.
Step 4: the raw materials react and then are deposited into a film in a chamber at room temperature.
Embodiments of the present disclosure will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are merely illustrative of the present disclosure and should not be construed as limiting the scope of the present disclosure. The perrelin used in the examples below is dichoro-p-cyclophane and Di-p-xylene [2,2] paracyclophane produced in the united states. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The parylene C material was removed from the vacuum drying tank and weighed into an evaporation chamber. After the cracking chamber is heated to 690 ℃, the evaporating chamber is heated to 175 ℃, the parylene C raw material is evaporated and then subjected to chemical reaction in the cracking chamber, then deposited on a substrate to form a film in a room temperature chamber, and the raw material which cannot be deposited is adhered to a cold well rod at low temperature through a cold well to prevent the raw material from entering a vacuum pump. The substrate is a common glass sheet.
Example 2
The parylene N feedstock was removed from the vacuum drying tank and weighed into an evaporation chamber. After the cracking chamber is heated to 650 ℃, the evaporating chamber is heated to 175 ℃, the parylene N raw material is evaporated and then subjected to chemical reaction in the cracking chamber, then deposited on a substrate to form a film in a room temperature chamber, and the raw material which cannot be deposited is adhered to a cold well rod at low temperature through a cold well to prevent the raw material from entering a vacuum pump. The substrate is a common glass sheet.
Example 3
Taking the parylene C raw material out of the vacuum drying tank, and weighing the required weight; and weighing the perfluorononane according to a certain mass-to-volume ratio. If the difference between the evaporation temperatures of the two raw materials is less than 10 ℃, the two raw materials can be mixed and placed into an evaporation chamber; if the difference between the evaporating temperatures of the two raw materials is more than 10 ℃, the two raw materials are required to be separately placed into an evaporating chamber. After the cracking chamber is heated to 690 ℃, the evaporating chamber is heated to 175 ℃, the parylene C and the fluorine-containing reagent are subjected to chemical reaction in the cracking chamber after being evaporated, then the film is deposited on the substrate in the chamber at room temperature, and the raw materials which cannot be deposited are adhered to a cold well rod at low temperature through a cold well to prevent the raw materials from entering a vacuum pump. The substrate is a common glass sheet.
Example 4
Taking the parylene N raw material out of the vacuum drying tank, and weighing the required weight; and weighing the perfluorononane according to a certain mass-to-volume ratio. If the difference between the evaporation temperatures of the two raw materials is less than 10 ℃, the two raw materials can be mixed and placed into an evaporation chamber; if the difference between the evaporating temperatures of the two raw materials is more than 10 ℃, the two raw materials are required to be separately placed into an evaporating chamber. After the cracking chamber is heated to 650 ℃, the evaporating chamber is heated to 175 ℃, the parylene N and the fluorine-containing reagent are subjected to chemical reaction in the cracking chamber after being evaporated, then the film is deposited on the substrate in the chamber at room temperature, and raw materials which cannot be deposited are adhered to a cold well rod at low temperature through a cold well to prevent the raw materials from entering a vacuum pump. The substrate is a common glass sheet.
Example 5
Taking the parylene C raw material out of the vacuum drying tank, and weighing the required weight; and weighing the perfluorononane according to a certain mass-to-volume ratio. If the difference between the evaporation temperatures of the two raw materials is less than 10 ℃, the two raw materials can be mixed and placed into an evaporation chamber; if the difference between the evaporating temperatures of the two raw materials is more than 10 ℃, the two raw materials are required to be separately placed into an evaporating chamber. After the cracking chamber is heated to 690 ℃, the evaporating chamber is heated to 175 ℃, the parylene C and the fluorine-containing reagent are subjected to chemical reaction in the cracking chamber after being evaporated, then the film is deposited on the substrate in the chamber at room temperature, and the raw materials which cannot be deposited are adhered to a cold well rod at low temperature through a cold well to prevent the raw materials from entering a vacuum pump. The substrate is a silicon wafer/PDMS with a nano structure.
Example 6
Taking the parylene N raw material out of the vacuum drying tank, and weighing the required weight; and weighing the perfluorononane according to a certain mass-to-volume ratio. If the difference between the evaporation temperatures of the two raw materials is less than 10 ℃, the two raw materials can be mixed and placed into an evaporation chamber; if the difference between the evaporating temperatures of the two raw materials is more than 10 ℃, the two raw materials are required to be separately placed into an evaporating chamber. After the cracking chamber is heated to 650 ℃, the evaporating chamber is heated to 175 ℃, the parylene N and the fluorine-containing reagent are subjected to chemical reaction in the cracking chamber after being evaporated, then the film is deposited on the substrate in the chamber at room temperature, and raw materials which cannot be deposited are adhered to a cold well rod at low temperature through a cold well to prevent the raw materials from entering a vacuum pump. The substrate is a silicon wafer/PDMS with a nano structure.
Fig. 2 shows a cross-section of a low surface energy parylene material of example 5 of the present invention in a porous structure. The parylene material with low surface energy provided by the invention is flat and compact, and the section is of a porous structure. The surface energy is reduced while the excellent physical and chemical properties of the original parylene material are maintained, and the contact angle is greatly improved.
Fig. 3 is the results of contact angle test experiments for samples of low surface energy parylene materials of the present invention. The samples prepared in examples 1-6, numbered samples S1-S6 in sequence, were used for contact angle experimental testing.
Comparative 6 sets of sample contact angle experimental data:
sample S1: unstructured modified pre-parylene C film (sample prepared in example 1);
sample S2: unstructured modified pre-parylene N film (sample prepared in example 2);
sample S3: unstructured modified parylene C film (sample prepared in example 3);
sample S4: unstructured modified parylene N film (sample prepared in example 4);
sample S5: modified parylene C film (sample prepared in example 5) overlaid on the nanostructure;
sample S6: modified parylene N film (sample prepared in example 6) overlaid on the nanostructure;
samples prepared in examples 1-4 were taken and numbered as samples S1-S4 in sequence, and tested for dielectric constant and mechanical properties, and the statistical data are shown in Table 1 below and FIG. 4:
TABLE 1 experimental results of dielectric constants for samples S1-S4
Compared with the original parylene raw material, the modified parylene material has lower surface energy, lower dielectric constant and certain improvement on mechanical property.
While the features of the invention have been shown and described in detail with reference to preferred embodiments, those skilled in the art will appreciate that other changes can be made therein without departing from the spirit of the scope of the invention. Likewise, the various figures may depict an example architecture or other configuration for the present disclosure for understanding the features and functionality that may be included in the present disclosure. The disclosure is not limited to the example architectures or configurations shown, but can be implemented using a variety of alternative architectures and configurations. Additionally, while the present disclosure has been described above in terms of various exemplary embodiments and implementations, it is to be understood that the various features and functions described in the context of one or more individual embodiments are not limited in their applicability to the particular embodiment to which they pertain. Rather, they may be applied to one or more other embodiments of the present disclosure, alone or in some combination, whether or not such embodiments are described and whether or not these features are presented as part of the described embodiments. Thus, the breadth and scope of the present disclosure should not be limited by any of the above-described exemplary embodiments.
Fig. 4 is the results of mechanical property testing experiments for samples of low surface energy parylene materials of the present invention.
Claims (7)
1. A low surface energy parylene material characterized by: is formed by chemical vapor deposition of a parylene raw material and a fluorine-containing reagent, the fluorine-containing reagent comprises 2,3, 4,5, 6, 7-dodecafluoro-1, 8-octanediol, 3-trifluoro ethyl propionate nine-carbon perfluoro polyether siloxane, 2-trifluoro ethyl ester perfluoropolyether, 2-trifluoroacetamide, perfluorononane, perfluorodecyl ethyl acrylate, undec fluoro-n-hexane-1-ol, perfluorodecane.
2. The low surface energy parylene material of claim 1, wherein: the difference between the evaporation temperature of the parylene raw material and the evaporation temperature of the fluorine-containing reagent is 0-25 ℃.
3. The low surface energy parylene material of claim 1, wherein: the cleavage temperature of the fluorine-containing reagent is below 700 ℃.
4. A method for preparing a low surface energy parylene material according to claim 1, comprising the steps of:
step 1, placing a parylene raw material and a fluorine-containing reagent into an evaporation chamber;
step 2, vacuumizing the whole reaction device to ensure that the reaction occurs under the vacuum condition;
step 3, firstly raising the temperature of the cracking furnace to 690 ℃ or 650 ℃, and then raising the temperature of the evaporating chamber to 175 ℃;
and 4, depositing a film on the substrate in the room temperature chamber after the raw materials react.
5. The method for preparing the low-surface-energy parylene material according to claim 4, wherein the method comprises the following steps: in said step 1, if the evaporation temperatures of the parylene feedstock and the fluorogenic agent differ by >10 ℃, the parylene feedstock and the fluorogenic agent should be placed separately into the evaporation chamber; if the evaporation temperatures of the parylene material and the fluorine-containing reagent differ by <10 ℃, the parylene material and the fluorine-containing reagent are mixed and placed into an evaporation chamber.
6. The method for preparing the low-surface-energy parylene material according to claim 4, wherein the method comprises the following steps: the base material adopts a metal base plate and needs to be subjected to adhesion performance enhancing treatment.
7. The method for preparing the low-surface-energy parylene material according to claim 4, wherein the method comprises the following steps: the raw materials which cannot be deposited in the step 4 are adhered to a cold well rod at a low temperature through a cold well, and are prevented from entering a vacuum pump.
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| CN115491653B (en) * | 2022-08-09 | 2023-10-27 | 电子科技大学(深圳)高等研究院 | Method for preparing hydrophobic film by chemical vapor deposition with temperature gradient regulation |
| CN115350886B (en) * | 2022-09-15 | 2024-04-19 | 上海派拉纶生物技术股份有限公司 | Composite protective coating, preparation method thereof and electronic device |
| CN117187773B (en) * | 2023-11-03 | 2024-03-08 | 上海锐畅医疗科技有限公司 | Hydrophilic coating for interventional medical instrument and preparation method thereof |
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