CN113105704A - Organic planar target material and preparation method thereof - Google Patents
Organic planar target material and preparation method thereof Download PDFInfo
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- CN113105704A CN113105704A CN202110344325.1A CN202110344325A CN113105704A CN 113105704 A CN113105704 A CN 113105704A CN 202110344325 A CN202110344325 A CN 202110344325A CN 113105704 A CN113105704 A CN 113105704A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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Abstract
The invention discloses an organic planar target material and a preparation method thereof, wherein the preparation method comprises the following steps: carbon Nanotube (CNT) powder and Polytetrafluoroethylene (PTFE) powder were pre-mixed into CNT: the weight ratio of PTFE is 1: 99,3: 97,5: 95, 10: 90, 15: 85, respectively. Mixing graphite powder and PTFE powder in a ratio of 15: 85. 30: 70, preparing a composite target material with carbon content higher than that of CNT/PTFE, preparing PTFE mixed powder with acetylene black volume fraction of 0.4%, preparing a CNT (graphite/carbon black)/PTFE composite polymer target material by a cold pressing sintering method, then milling and welding a back plate, wherein the diameter and the height of the prepared target material are not limited, and the process parameters are as follows: the preforming pressure is 14.71-29.4 MPa, the pressure is maintained for about 10min, the sintering temperature is above 327 ℃, the organic composite target material has good conductivity, medium-frequency current (MF) can be used for magnetron sputtering, the efficiency is high, and the fluorocarbon film prepared by the target material has good light transmittance and hydrophobicity, low surface energy, and high hardness and modulus.
Description
Technical Field
The invention relates to the technical field of targets and target preparation, in particular to an organic planar target and a preparation method thereof.
Background
The organic target material is suitable for the fields of flat panel display, flexible display, automobile, textile fiber, electronic equipment and the like, and the organic target material is required to have the advantages of high purity, high density, large-size integration and the like.
At present, the PTFE target is mainly prepared by using a pre-formed powder and thermocompression bonding, and considering that an organic material is non-conductive, RF sputtering is widely used when a thin film is deposited using an insulating material, but this method has high cost, low productivity, and difficulty in applying to a large-area substrate, so to solve this problem, CNT or graphite powder or carbon black is mixed into PTFE powder to make the target conductive, so that it is possible to deposit an insulating film using an intermediate frequency (MF) sputtering method using a conductive target instead of RF sputtering.
In order to meet higher coating requirements, a new technology for preparing a high-performance organic target material is urgently needed.
In order to solve the problems, the scheme is developed accordingly.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides an organic planar target and a preparation method thereof, and solves the problems in the background art.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: an organic composite target is characterized in that the thickness is 3-15 mm, the relative density of the target is more than or equal to 97%, the purity is more than or equal to 99.99%, the oxygen content is less than or equal to 200ppm, the content of carbon element is 1-30 wt%, and the balance is PTFE.
The method comprises the following steps:
step 1, pretreatment of resin;
step 2, sieving the resin;
step 3, mixing the powder;
step 4, preforming;
step 5, sintering;
step 6, milling and forming;
and 7, connecting the back plate.
In step 1, the temperature of the PTFE powder is adjusted before molding, by placing the resin in a container, placing the container in an environment of 23-25 deg.C, and standing for 24-48 h, wherein the pre-molding is performed at the temperature.
Preferably, the average particle size of the PTFE powder is 150-250 microns; the method is characterized in that reagent-grade graphite particles are not more than 30um, the residue content is less than 0.15%, the moisture content is less than 0.5%, the relative density is 2.09-2.25, and the particle size of carbon black is 20 um.
Preferably, in the step 2, a 10-20-mesh sieve is used for sieving before use, and impurities are strictly forbidden to be introduced in the sieving process so as to prevent the product performance from being influenced.
Preferably, in the step 3, dry mixing is adopted, a certain amount of PTFE powder is weighed, the PTFE powder is added into a pot of a high-speed mixer, a cover is closed, the stirring is carried out for 0.5-1 min, the resin is loosened, the stirring is stopped, a filling agent is added according to a formula and the cover is closed, a stirrer is started, the stirring is carried out for 2-8 min, the material is discharged under the stirring condition, the stirring and mixing effect is related to the stirring speed, the stirring time, the formula amount and the physical properties, heat is generated during the high-speed mixing, a jacket layer is arranged on a mixing pot, cooling can be carried out through cooling water, and the material in the pot is not influenced.
The average particle size of PTFE powder is 150-250 microns; the method adopts the technical scheme that the particle size of reagent-grade graphite is not more than 30um, the residue content is less than 0.15 percent, the moisture content is less than 0.5 percent, the relative density is 2.09-2.25, and the particle size of carbon black is 20um
Preferably, in the step 4, multiple-layer molding is adopted, during feeding, prepared raw materials are weighed according to the size of a workpiece, the raw materials are added into a cleaned mold cavity, resin in the mold cavity of a metal scraper target is spread, the resin is uniformly distributed in the mold cavity, firstly, a release agent is required to be added to the cleaned mold before preforming, the release agent is prepared from 1 part of absolute ethyl alcohol and 1 part of phenol, and an organic silicon release agent can also be adopted; secondly, when the feeding is carried out in a multiple feeding mode, the material is compressed by slightly pressurizing after each feeding so as to facilitate the next feeding, and the pressure is required to be 30kgf/cm2In the following, excessive pressure may form a layer between the charges, often causing cracks in the product; thirdly, the feeding environment needs to be clean, and feeding needs to be fast, so that dust in the air is prevented from entering the product; during pressing, after adding materials, closing the die, slowly applying pressure, not allowing impact type pressurization, paying attention to thicker products, releasing pressure for 2-4 times in the pressure boosting process, preferably lowering the male die at a speed of 30-50 mm/min, boosting pressure at a speed of a few millimeters per minute near the final pressure, and removing the cushion block when boosting pressure to two thirds of the specified pressure to enable the preform to be pre-formedExtruding the two sides of the shaped product, keeping pressure for about 10min after sufficient pressure is applied, ensuring uniform pressure transmission, enough pressure keeping time, then slowly releasing the pressure, taking the preformed product out of the film cavity, wherein the preformed pressure is different according to the size and the temperature of particles, releasing the pressure during demolding, carefully taking the preformed product out, wherein large vibration and sudden external force impact are not allowed, fully considering the compression ratio and the shrinkage ratio during pressing, adopting a fused deposition manufacturing technology for molding, manufacturing the mixed material into a wire material by a pushing and pressing method, firstly winding the wire material on a feeding roller, heating the wire-shaped hot-melting material by a resistance wire type heater arranged on a nozzle, extruding the molding material by the nozzle after the wire material is melted into a semi-liquid state, selectively coating the molding material on a worktable, arranging a low-friction guide sleeve between the feeding roller and the nozzle, and ensuring that the wire material can be smoothly and accurately fed into the inner cavity of the nozzle by the feeding roller, the nozzle can move along the X-Y plane, the molten wire is extruded and coated on the material of the upper layer, the working platform is lowered by a thickness according to the increment set by the system after the deposition of one layer of molding material is finished, and the process is circulated until the three-dimensional part product is formed.
Preferably, in step 5, the preform product is heated to above 327 ℃ of the melting point of the PTFE crystal, and is kept for a suitable time to gradually change the polymer molecule crystal into an amorphous form, the dispersed single resin particles are mutually diffused, melted and bonded into a continuous whole, and finally cooled to gradually change the polymer molecule from the amorphous form into the crystal, and in the cooling process, products with different degrees of crystallinity can be obtained by changing the cooling mode, and the sintering process is the most important link in the whole process. All the preformed products are sintered to make the products have strength and use value. An indirect sintering method is adopted and comprises three stages of heating, sintering (heat preservation) and cooling, and during heating, the temperature is raised at a speed of 60-70 ℃/h; another heating mode is heating in stages, and the temperature is gradually increased to about 380 ℃ by heat preservation, which is determined after comprehensive analysis of factors such as the size, the shape, the grade of raw materials and the like of a product. The heat preservation and sintering temperature are key data for ensuring the product quality, and operators must carefully and strictly control the operation. The sintering temperature of the suspension polymerization resin is 370-380 ℃: the sintering temperature of the suspension polymer product with the average particle size of 150-250 mu m is 375 +/-5 ℃; the sintering temperature of a suspension polymer product with the average particle size of 25-50 mu m is (375 +/-59) DEG C, the heat preservation time is determined by the size of a preformed product and the particle size of the selected resin, the heat preservation time of a general large-sized product is 5-10 h, the heat preservation time of a small-sized product is 1h, the heat preservation time of a fine particle size PTFE resin preformed product is different from the heat preservation time of a coarse particle preformed product, and the cooling speed is 30-40 ℃/h; because of different cooling speeds and different crystallinity of the product, the performance of the product is different, and the sample formed by fused deposition should be subjected to pressure sintering to enhance the compactness.
Preferably, in step 6, the machining process generates heat, even softens and deforms the material, and affects the dimensional accuracy or quality of the parts, so that cooling water (soap water cooling) must be used, and the milling process is not fast enough, and the generated heat is lower than the softening point temperature of the target material.
Preferably, in step 7, a hot-press welding process can be adopted, a layer of PFA is added between the copper back plate and the target material, the copper back plate and the target material are welded together, the welding temperature is 370-380 ℃, and the welding pressure is controlled at 20kgf/cm2In the following, there is a direct relationship between pressure and temperature, and the weld strength and holding time are related to the heating temperature. The PTFE target is bonded by using an adhesive, and before bonding, surface treatment is required, and cleaning is generally performed by surface cleaning with water, alcohol, or an acetone-based solvent, and drying to obtain a clean bonding surface. The surface treatment refers to a surface chemical or physical treatment of the surface to which PTFE is bonded. Some common treatment methods include sodium-naphthalene chemical treatment, glow discharge method, boric acid liquid laser treatment, irradiation grafting method, alkali liquor reflux method and the like, and the sodium-Cai chemical treatment method is commonly used in the current production. The adhesive is widely available, and silicone adhesive, epoxy adhesive, acetal adhesive, urethane adhesive, and the like are used. According to the material and practical application of the adherendThe selection is required. It should be noted that the adhesion fastness of adhesives with fluoroplastics does not require as much fastness as welding and other mechanical connections.
(III) advantageous effects
After adopting the technical scheme, compared with the prior art, the invention has the following advantages:
according to the organic composite target material, the PTFE organic composite target material doped with the CNT/graphite has high purity, high density and good conductivity, the target material prepared by doping the CNT/graphite is a target material with good conductivity, intermediate-frequency current sputtering can be used, the cost is saved, the efficiency is improved, and meanwhile, the problems that the cost is high, the production efficiency is low and the application to a large-area substrate is difficult due to the fact that a single PTFE organic target material can only be subjected to radio frequency sputtering are solved. In addition, the forming equipment is simple to operate, the number of operators is small, the repeatability is good, and the target material cost can be effectively reduced.
According to the preparation method of the organic composite target material, when the target material is prepared by a sintering process, the sintering temperature is higher than the melting temperature (327 ℃) of the PTFE material, the target material is always in a molten state, the PTFE and the CNT/graphite are better fused, the porosity of the target material is reduced, and the density of the target material can be effectively ensured.
Detailed Description
The present invention is further illustrated in detail by the following examples
The basic preparation process of the organic composite target material of the invention is as follows
(1) Pretreatment of resin: placing PTFE in an environment with the temperature of 23-25 ℃ for 24-48 h;
(2) sieving the resin: sieving PTFE powder by using a sieve with 10-20 meshes before use;
(3) powder mixing: mixing by adopting a dry method;
(4) preforming: a layered multiple forming or fused deposition forming technology is adopted;
(5) and (3) sintering: adopting an indirect sintering method, wherein the temperature is higher than 327 ℃;
(6) milling and forming: molding the product by a milling machine, and cooling;
(7) and connecting the back plate.
Example 1
The embodiment is a preparation method of an organic composite target, which comprises the following steps:
(1) powder pretreatment: placing PTFE in an environment of 23-25 ℃ for 24-48 h, sieving PTFE powder with a 10-20-mesh sieve before use, selecting CNT and PTFE powder, and mixing the materials in a mass ratio of 1: 99 CNT and PTFE powder are dispersed in a container.
(2) Powder premixing: fully and uniformly mixing CNT and PTFE powder;
(3) molding: and (3) performing compression molding on the CNT powder and the PTFE powder which are fully and uniformly mixed by adopting a layering and multi-time molding process. The specific parameters are as follows: the compression pressure is 14.71-29.4 MPa, the pressing time is 10min, and the temperature is 23-25 ℃;
(4) and (3) sintering: sintering at 370-380 deg.c, maintaining for 1 hr and cooling.
(5) Milling and forming: and milling and forming the blank formed by hot pressing by a milling machine, wherein the radius is 4-10 cm, and the thickness is 3-15 mm.
(6) And connecting the back plate.
The performance of the target material is analyzed by using a scanning electron microscope, a metallographic microscope, a high-precision electronic scale and a mutual inductance coupling plasma mass spectrometer (ICP), the thickness of the organic composite target material prepared by the embodiment is 5mm, the relative density is 98%, the porosity is less than or equal to 1.9%, and the average grain size is less than 150 microns.
Example 2
The embodiment is a preparation method of an organic composite target, which comprises the following steps:
(1) powder pretreatment: placing PTFE in an environment of 23-25 ℃ for 24-48 h, sieving PTFE powder with a 10-20-mesh sieve before use, selecting CNT and PTFE powder, and mixing the materials in a mass ratio of 5: 95 CNT and PTFE powder were dispersed in a container.
(2) Powder premixing: fully and uniformly mixing CNT and PTFE powder;
(3) molding: and (3) performing compression molding on the CNT powder and the PTFE powder which are fully and uniformly mixed by adopting a layering and multi-time molding process. The specific parameters are as follows: the compression pressure is 14.71-29.4 MPa, the pressing time is 10min, and the temperature is 23-25 ℃;
(4) and (3) sintering: sintering at 370-380 deg.c, maintaining for 1 hr and cooling.
(5) Milling and forming: and milling and forming the blank formed by hot pressing by a milling machine, wherein the radius is 4-10 cm, and the thickness is 3-15 mm.
(6) And connecting the back plate.
The performance of the target material is analyzed by using a scanning electron microscope, a metallographic microscope for analysis, a high-precision electronic scale and a mutual inductance coupling plasma mass spectrometer (ICP), the thickness of the organic composite target material prepared by the embodiment is 8mm, the relative density is 97.8%, the porosity is less than or equal to 2%, and the average grain size is less than 150 microns.
Example 3
The embodiment is a preparation method of an organic composite target, which comprises the following steps:
(1) powder pretreatment: placing PTFE in an environment of 23-25 ℃ for 24-48 h, sieving PTFE powder with a 10-20-mesh sieve before use, selecting CNT and PTFE powder, and mixing the materials in a mass ratio of 10: 90 CNT and PTFE powder were dispersed in a container.
(2) Powder premixing: fully and uniformly mixing CNT and PTFE powder;
(3) molding: and (3) performing compression molding on the CNT powder and the PTFE powder which are fully and uniformly mixed by adopting a layering and multi-time molding process. The specific parameters are as follows: the compression pressure is 14.71-29.4 MPa, the pressing time is 10min, and the temperature is 23-25 ℃;
(4) and (3) sintering: sintering at 370-380 deg.c, maintaining for 1 hr and cooling.
(5) Milling and forming: and milling and forming the blank formed by hot pressing by a milling machine, wherein the radius is 4-10 cm, and the thickness is 3-15 mm.
(6) And connecting the back plate.
The performance of the target material is analyzed by using a scanning electron microscope, a metallographic microscope, a high-precision electronic scale and a mutual inductance coupling plasma mass spectrometer (ICP), the thickness of the organic composite target material prepared by the embodiment is 10mm, the relative density is 97.5%, the porosity is less than or equal to 2.2%, and the average grain size is less than 150 microns.
Example 4
The embodiment is a preparation method of an organic composite target, which comprises the following steps:
(1) powder pretreatment: placing PTFE in an environment of 23-25 ℃ for 24-48 h, sieving PTFE powder with a 10-20-mesh sieve before use, selecting CNT and PTFE powder, and mixing the materials in a mass ratio of 15: 85 of CNT and PTFE powder are dispersed in a container.
(2) Powder premixing: fully and uniformly mixing CNT and PTFE powder;
(3) molding: and (3) performing compression molding on the CNT powder and the PTFE powder which are fully and uniformly mixed by adopting a layering and multi-time molding process. The specific parameters are as follows: the compression pressure is 14.71-29.4 MPa, the pressing time is 10min, and the temperature is 23-25 ℃;
(4) and (3) sintering: sintering at 370-380 deg.c, maintaining for 1 hr and cooling.
(5) Milling and forming: and milling and forming the blank formed by hot pressing by a milling machine, wherein the radius is 4-10 cm, and the thickness is 3-15 mm.
(6) And connecting the back plate.
The performance of the target material is analyzed by using a scanning electron microscope, a metallographic microscope, a high-precision electronic scale and a mutual inductance coupling plasma mass spectrometer (ICP), the thickness of the organic composite target material prepared by the embodiment is 12mm, the relative density is 97%, the porosity is less than or equal to 2.5%, and the average grain size is less than 150 microns.
Example 5
The embodiment is a preparation method of an organic composite target, which comprises the following steps:
(1) powder pretreatment: placing PTFE in an environment of 23-25 ℃ for 24-48 h, sieving PTFE powder with a 10-20-mesh sieve before use, selecting graphite powder and PTFE powder, and mixing the materials in a mass ratio of 15: 85 of graphite powder and PTFE powder are dispersed in a container.
(2) Powder premixing: fully and uniformly mixing graphite powder and PTFE powder;
(3) molding: and (3) compressing and molding the graphite powder and the PTFE powder which are fully and uniformly mixed by adopting a layered multi-time molding process. The specific parameters are as follows: the compression pressure is 14.71-29.4 MPa, the pressing time is 10min, and the temperature is 23-25 ℃;
(4) and (3) sintering: sintering at 370-380 deg.c, maintaining for 1 hr and cooling.
(5) Milling and forming: and milling and forming the blank formed by hot pressing by a milling machine, wherein the radius is 4-10 cm, and the thickness is 3-15 mm.
(6) And connecting the back plate.
The performance of the target material is analyzed by using a scanning electron microscope, a metallographic microscope for analysis, a high-precision electronic scale and a mutual inductance coupling plasma mass spectrometer (ICP), the thickness of the organic composite target material prepared by the embodiment is 9mm, the relative density is 97.6%, the porosity is less than or equal to 2%, and the average grain size is less than 150 microns.
In light of the foregoing, it will be apparent to those skilled in the art from this disclosure that various changes and modifications can be made without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and the protection scope must be determined by the scope of the claims.
Claims (9)
1. An organic composite target material is 3-15 mm thick, the relative density of the target material is more than or equal to 97%, the purity of the target material is more than or equal to 99.99%, the oxygen content is less than or equal to 200ppm, the content of carbon element is 1-30 wt%, and the balance is PTFE.
2. A preparation method of an organic composite target material comprises the following steps:
step 1, pretreatment of resin;
step 2, sieving the resin;
step 3, prefabricating CNT/graphite/carbon black and PTFE mixed powder, and uniformly mixing the CNT/graphite/carbon black and PTFE mixed powder;
step 4, performing the prefabricated mixed powder;
step 5, sintering;
step 6, milling and forming;
and 7, connecting the back plate.
3. The method according to claim 2, wherein in step 1, the temperature of the PTFE powder is adjusted before molding by charging the resin to be used in a container, placing the container in an environment of 23 to 25 ℃ and standing for 24 to 48 hours, and performing the preforming at the temperature.
4. The method for preparing the organic composite target material according to claim 2, wherein in the step 2, the PTFE powder is sieved through a 10-20-mesh sieve before use, and introduction of impurities is strictly prohibited during sieving.
5. The method of claim 2, wherein in step 3, the CNT/graphite/carbon black and PTFE powder are characterized as follows: the average particle size of PTFE powder is 150-250 microns; reagent-grade graphite particles are not more than 30um, the residue content is less than 0.15%, the moisture content is less than 0.5%, the relative density is 2.09-2.25, and the particle size of carbon black is 20 um;
the mixing mode adopts dry mixing: weighing a certain amount of PTFE powder, adding the PTFE powder into a pot of a high-speed mixer, covering the pot, stirring for 0.5-1 min to loosen resin, stopping stirring, adding a filling agent according to a formula, covering the filling agent, starting a stirrer, stirring for 2-8 min, and discharging under the stirring condition, wherein the mixing pot is provided with a jacket layer and is cooled by cooling water.
6. The method for preparing the organic composite target material according to claim 2, wherein in the step 4, the CNT/graphite/carbon black powder and the PTFE powder are subjected to temperature control and pressurization, the compression pressure is 14.71-29.4 MPa, the temperature is 23-25 ℃, and the pressing time is 10 min;
the preforming is layered and repeatedly molded, when the materials are added, prepared raw materials are weighed according to the size of a workpiece and added into a cleaned die cavity, and resin in the die cavity is paved by using a metal scraper target, so that the resin is uniformly distributed in the die cavity;
the attention point of feeding is that 1, a mold cleaned in feeding needs to be provided with a release agent before preforming, and the release agent is prepared by 1 part of absolute ethyl alcohol and 1 part of phenol or is an organic silicon release agent; 2. when the feeding is carried out in a multiple feeding mode, the materials are compressed by pressurizing after each feeding so as to facilitate the feeding at the next time,the pressure was controlled to 30kgf/cm2The following; 3. the feeding environment is kept clean, and the feeding is carried out quickly, so that dust in the air is prevented from entering the product;
during pressing, after materials are added, closing a die, slowly applying pressure, not allowing impact type pressurization, paying attention to a thicker product, releasing pressure for 2-4 times in the pressure boosting process, enabling a male die to descend at a speed of 30-50 mm/min, boosting the pressure at a speed of several millimeters per minute when the pressure is close to the final pressure, removing a cushion block when the pressure is boosted to two thirds of the specified pressure, extruding two sides of the preformed product, maintaining the pressure for about 10 minutes after the pressure is fully exerted, ensuring that the pressure is uniformly transmitted and has enough pressure maintaining time, slowly releasing the pressure, taking the preformed product out of a film cavity, wherein the preformed pressure is different along with the size and the temperature of particles;
during demolding, after decompression, the preformed product is taken out and protected from being shocked by vibration and force, and the material is made into wire through extrusion, winding the wire around the feeding roller, heating the wire with electric resistance wire heater in the nozzle, extruding and coating the material onto the bench selectively after the wire is molten into semi-liquid state, setting one guide sleeve with low friction force between the feeding roller and the nozzle, moving the nozzle along X-Y plane, extruding the molten wire and coating the material onto the upper layer, lowering the bench by one thickness based on the increment set in the system after depositing one layer of material, and repeating the steps until forming three-dimensional part product.
7. The method according to claim 2, wherein in step 5, the preformed product is heated to a temperature above 327 ℃ of the melting point of the PTFE crystal, left to stand, the polymer molecule is gradually changed into amorphous form, the dispersed individual resin particles are mutually diffused, melted and bonded into a continuous whole, and finally cooled to gradually change the polymer molecule from amorphous form into crystalline form, and the cooling mode is changed during the cooling process to obtain products with different degrees of crystallinity;
heating at a speed of 60-70 ℃/h by adopting an indirect sintering method; or another heating mode of heating by stages is adopted, and the temperature is gradually increased to 380 ℃; the sintering temperature of the suspension polymer resin is 370-380 ℃, the sintering temperature of the suspension polymer product with the average grain diameter of 150-250 μm is 375 +/-5 ℃; the sintering temperature of the suspension polymer product with the average particle size of 25-50 mu m is 375 +/-59 ℃; wherein the heat preservation time of the large-sized product is 5-10 h, the heat preservation time of the small-sized product is 1h, and the cooling speed is 30-40 ℃/h.
8. The method for preparing the organic composite target material according to claim 2, wherein in the step 6, the formed sample is milled and shaped into a round cake shape with a diameter of 4-10 cm and a thickness of 3-15 mm by using a milling machine, and is cooled by using cooling water or soap water, and the speed is controlled during milling to realize that the generated heat is lower than the softening point temperature of the target material.
9. The method for preparing the organic composite target material according to claim 2, wherein in the step 7, a hot-press welding process or an adhesive bonding process is adopted: adding a layer of PFA between the copper back plate and the target material, welding the copper back plate and the target material together, wherein the welding temperature is 370-380 ℃, and the welding pressure is controlled at 20kgf/cm2The following, the binder bonding: before bonding, surface treatment is carried out, namely surface cleaning and drying are carried out by adopting water, alcohol and acetone solvents to obtain a clean bonding surface, the bonding surface of the PTFE target is chemically or physically treated, and the contact surface of the bonded copper plate is also subjected to physical treatment of cleaning, drying and roughening modes.
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| CN202110344325.1A CN113105704A (en) | 2021-03-31 | 2021-03-31 | Organic planar target material and preparation method thereof |
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| CN202110344325.1A Pending CN113105704A (en) | 2021-03-31 | 2021-03-31 | Organic planar target material and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107208254A (en) * | 2015-01-28 | 2017-09-26 | 韩国化学研究院 | Sputtering fluorine class macromolecule composition target |
| KR20170138722A (en) * | 2016-06-08 | 2017-12-18 | 한국화학연구원 | Adhesion method of fluoropolymer composite target for deposition and devices formed therefrom |
| CN108943779A (en) * | 2018-08-27 | 2018-12-07 | 四川大学 | A kind of preparation method of high filler loading PTFE composite membrane material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107208254A (en) * | 2015-01-28 | 2017-09-26 | 韩国化学研究院 | Sputtering fluorine class macromolecule composition target |
| KR20170138722A (en) * | 2016-06-08 | 2017-12-18 | 한국화학연구원 | Adhesion method of fluoropolymer composite target for deposition and devices formed therefrom |
| CN108943779A (en) * | 2018-08-27 | 2018-12-07 | 四川大学 | A kind of preparation method of high filler loading PTFE composite membrane material |
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