CN110791727A - Wear-resistant coating for polyimide film stretcher and preparation method thereof - Google Patents
Wear-resistant coating for polyimide film stretcher and preparation method thereof Download PDFInfo
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- CN110791727A CN110791727A CN201911201855.XA CN201911201855A CN110791727A CN 110791727 A CN110791727 A CN 110791727A CN 201911201855 A CN201911201855 A CN 201911201855A CN 110791727 A CN110791727 A CN 110791727A
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
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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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/129—Flame spraying
Abstract
The invention relates to a wear-resistant coating for a polyimide film stretcher and a manufacturing method thereof, wherein the wear-resistant coating for the polyimide film stretcher contains 85-95% of zirconium oxide. The invention solves the problem that the polyimide film is polluted due to the fact that metal filings fall off because metal needles used for fixing the film are abraded in the polyimide film manufacturing process from the source, namely, the abrasion-resistant coating can prevent the polyimide film from being polluted by the metal filings in the batch production process, the film can be kept highly clean without being washed, and the polyimide film is beneficial to batch and continuous production.
Description
Technical Field
The invention relates to the technical field of heat-resistant and wear-resistant coatings, in particular to a wear-resistant coating for a polyimide film stretcher and a preparation method thereof.
Background
With the vigorous development of science and technology and industrial technology, the polyimide film (PI) has the special properties of high strength, high toughness, high temperature resistance, wear resistance, corrosion resistance and the like, and particularly meets the design requirements of lightness and thinness, so that the PI is a high-temperature-resistant insulating material with competitive advantages.
In recent years, the manufacturing process of polyimide films is mature, the biaxial stretching technology of polyimide films tends to replace uniaxial stretching gradually, and the polyimide films are stretched in the longitudinal and transverse orthogonal directions in the manufacturing process to provide more uniform stress to the films, so that the elastic coefficient, the tearing strength and the tensile strength of the films can be improved accordingly.
In the existing polyimide biaxial stretching machine, a polyimide film which is not fully imidized is fixed on a metal needle of a needle plate type chain and passes through a high-temperature imidizing furnace synchronously with the needle plate type chain, so that the film is imidized and simultaneously exerts transverse and longitudinal stretching force on the film. However, the temperature in the high-temperature imidization furnace is as high as 300-400 ℃, polar aprotic solvents such as N-methylpyrrolidone, N '-dimethylacetamide and N, N' -dimethylformamide volatilize in the film imidization process, and the pin plate type chain passes through the high-temperature imidization furnace repeatedly in a circulating manner in such an environment, so that the metal pin is easily corroded at high temperature to generate abrasion and fall off fine metal chips, and the metal chips are left on the polyimide film and are extremely difficult to remove, thereby causing troubles to the production of the polyimide film. At present, most methods for solving the problem adopt a water washing mode, the polyimide film needs to be repeatedly washed, the removing effect is limited, and the batch production of the polyimide film is hindered.
Disclosure of Invention
The invention aims to overcome the defects and aims to solve the problem that metal scraps falling off from metal needles on a needle plate type chain due to corrosion and abrasion pollute a polyimide film from the source, so that the invention further provides a wear-resistant coating for a polyimide film stretcher and a preparation method thereof.
According to the technical scheme provided by the invention, the wear-resistant coating for the polyimide film stretcher can be provided, and the coating contains 85-95% of zirconium oxide.
In addition, the coating also contains 0.1-5% of boron nitride.
In addition, the balance of the coating is one or more of yttrium oxide, silicon oxide, aluminum oxide, scandium oxide, cerium oxide, titanium oxide, tin oxide and strontium oxide.
In addition, the thickness of the coating is 1-100 μm.
The invention also provides a manufacturing method of the wear-resistant coating, which comprises the following steps:
(1) cleaning the surface of the metal needle;
(2) drying the raw materials for the wear-resistant coating, uniformly mixing, and spraying the mixture on the surface of the metal needle;
(3) drying at room temperature.
Wherein the spraying comprises any one of supersonic flame spraying, plasma spraying, cold spraying, electric arc spraying and suspension spraying.
In addition, the spraying is plasma spraying, and the spraying parameters are as follows: the flow rate of main gas Ar is 60-65L/min, and the flow rate of auxiliary gas H2The flow rate is 10-12L/min, the flow rate of Ar of the powder feeding gas is 6-7L/min, the powder feeding rate is 15-20 g/min, the current is 500-600A, the gun swing speed is 500-600 mm/s, the spraying distance is 60-70 mm, and the spraying angle is 75-90 degrees.
In addition, the spraying is supersonic flame spraying, the used fuel gas is propane, the combustion-supporting gas is oxygen, the powder feeding gas is nitrogen, and the gas flow rates are respectively as follows: 80-90 mL/min propane, 200-400 mL/min oxygen and 20-80 mL/min nitrogen, the spraying distance is 60-70 mm, and the length of the spray pipe is 80-120 mm.
The step (1) is specifically as follows: the surface of the metal needle is washed clean by clean water, sand blasting is carried out until the surface roughness is more than 2.0 mu m, and then the surface of the metal needle is cleaned by absolute ethyl alcohol or acetone.
Further, the raw material for the abrasion-resistant coating layer has an average particle diameter of 0.01 to 5 μm.
The invention has the beneficial effects that: the invention solves the problem that the metal needle on the needle plate type chain is abraded and falls off metal scraps after being corroded in a high-temperature imide furnace so as to pollute the polyimide film from the source, so that the abrasion-resistant coating for the polyimide film stretcher can be coated on the metal needle, the polyimide film is not polluted by the metal scraps in the batch production process, the film can be kept highly clean without being washed, and the batch continuous production of the polyimide film can be promoted.
Detailed Description
The present invention is described more specifically by way of examples, but the present invention is not limited to these examples, and various modifications can be made by those skilled in the art within the technical spirit of the present invention.
In the present specification, the numerical range represented by "numerical value a to numerical value B" means a range including the end point numerical value A, B.
In the present specification, "%" denotes mass% unless otherwise specified.
In this specification, the abrasion-resistant coating for a polyimide film stretcher of the present invention is sometimes simply referred to as "corrosion-resistant coating", "corrosion-resistant abrasion-resistant coating" or "abrasion-resistant coating".
The polyimide film is prepared by reacting diamine and dibasic anhydride in a solvent with high boiling point and aprotic activity such as dimethylformamide, N-methylpyrrolidone and the like, and high-temperature imidization at 300-400 ℃ is needed in the polymerization process of the diamine and the dibasic anhydride. In order to impart better mechanical properties and heat shrinkage properties to a film, the film before imidization is generally fixed to a metal needle of a pin plate type chain, and passed through a high temperature imidization furnace in synchronization with the pin plate type chain to apply lateral and longitudinal tensile forces to the film while imidizing the film, thereby imparting better mechanical properties to the polyimide film. Therefore, in order to avoid the corrosion damage of the pin plate type chain when the pin plate type chain is subjected to high temperature and a high temperature imine furnace with solvent volatilization, a corrosion-resistant and wear-resistant coating is plated on the metal pin.
The corrosion-resistant and wear-resistant coating contains 85-95% of zirconia component. The zirconia material has excellent physical and chemical properties such as high hardness, high strength, high toughness, extremely high wear resistance, chemical corrosion resistance and the like. Wherein, the melting point of the zirconium oxide is 2680 ℃, the boiling point of 4300 ℃, the hardness of the zirconium oxide is inferior to that of diamond, and the zirconium oxide has extremely strong chemical corrosion resistance, so the zirconium oxide is particularly suitable for being used as a wear-resistant coating material in a high-temperature imine furnace. In addition, the content of the zirconia component is preferably 90 to 92% in terms of contributing to formation of a strong, thin, corrosion-resistant, and wear-resistant coating.
In addition, the coating also contains 0.1-5% of boron nitride, and the boron nitride is low in expansion coefficient, low in friction coefficient, good in high-temperature stability, high in strength and corrosion-resistant. Particularly, the boron nitride is doped in the corrosion-resistant and wear-resistant coating by 0.1-5%, plays roles in lubricating and neutralizing hardness, is beneficial to forming an ultrathin coating without cracking, and is particularly suitable for forming a coating on a metal needle of a polyimide stretcher. In addition, the content of boron nitride is preferably 1 to 3% in terms of facilitating the formation of a thin layer and preventing cracking of the coating layer.
In addition, the coating of the present invention may further contain one or more of yttrium oxide, silicon oxide, aluminum oxide, scandium oxide, cerium oxide, titanium oxide, tin oxide, and strontium oxide.
In the existing polyimide film stretcher, the diameter of a metal needle positioned on a needle plate type chain is less than 0.5mm, the thickness of a coating coated on the metal needle is preferably 1-100 mu m, if the coating is too thin, the adhesion of the coating and the metal needle is reduced, the coating is easy to fall off to pollute the polyimide film, if the coating is too thick, the fixing of the film is not facilitated, and if the coating is too thick, the transverse stretching of the film is influenced, and the film cannot be endowed with good transverse stretching force. In addition, the coating layer of the present invention is preferably 1 to 50 μm, more preferably 5 to 10 μm, in consideration of the adhesion of the coating layer and the transverse stretching of the film.
In addition, the present invention provides a method for producing the wear-resistant coating, comprising the steps of:
(1) cleaning the surface of the metal needle;
(2) drying the raw materials for the wear-resistant coating, uniformly mixing, and spraying the mixture on the surface of the metal needle;
(3) drying at room temperature.
The surface of the metal needle is cleaned, specifically, the surface of the metal needle is washed clean by clean water, sand blasting is carried out until the surface roughness is more than 2.0 mu m, and then the surface of the metal needle is cleaned by absolute ethyl alcohol or acetone. The surface of the metal needle is cleaned, which is beneficial to enhancing the adhesiveness between the wear-resistant coating and the metal needle, so that the coating is firmer and is prevented from falling off.
In the present invention, the wear-resistant coating material is preferably formed on the metal needle of the drawing machine by spray coating, which includes any one of supersonic flame spraying, plasma spraying, cold spraying, arc spraying, and suspension spraying. Among them, plasma spraying and supersonic flame spraying are preferable.
As plasma spraying, the spraying parameters are preferably: the flow rate of main gas Ar is 60-65L/min, and the flow rate of auxiliary gas H2The flow rate is 10-12L/min, the flow rate of Ar of the powder feeding gas is 6-7L/min, the powder feeding rate is 15-20 g/min, the current is 500-600A, the gun swing speed is 500-600 mm/s, the spraying distance is 60-70 mm, and the spraying angle is 75-90 degrees. Wherein, in order to make the formed coating more compact and enhance the adhesion with the metal needle, the main gas Ar flow is preferably 60-65L/min, and the auxiliary gas H is preferably2The flow rate is 10-12L/min, the flow rate of Ar of the powder feeding gas is 6-7L/min, and the powder feeding rate is 15-20 g/min. When the spraying distance is too large, the temperature and the speed of the powder particles are reduced, and the adhesive force and the spraying efficiency are influenced; the spraying distance is too small, so that the temperature of the metal needle is too high, the metal needle and the coating are oxidized, and the adhesive force is influenced, therefore, the spraying distance is preferably 60-70 mm. Too small a spray angle affects deterioration of the coating structure to cause loosening of the coating, and thus the spray angle is preferably 75 to 90 °. The moving speed of the spray gun is required to ensure that the coating is flat and no spraying ridge mark appears, and the higher moving speed of the spray gun is adopted as much as possible, so that local hot spots and surface oxidation can be prevented. Therefore, the preferred gun swing speed of the invention is 500-600 mm/s. As the supersonic flame spraying, it is preferable that the fuel gas used is propane, the combustion-supporting gas is oxygen, and the powder-feeding gas is nitrogen. Also, the gas flow rates thereof are preferably: 80-90 mL/min propane, 200-400 mL/min oxygen and 20-80 mL/min nitrogen, the spraying distance is 60-70 mm, and the length of the spray pipe is 80-120 mm.
In addition, the average particle size of the raw material for the abrasion-resistant coating layer of the present invention is 0.01 to 5 μm, more preferably 0.5 to 2 μm, in order to form a more uniform coating layer and to form a thinner layer and a coating layer having good adhesion in good combination with the parameters of plasma spraying and supersonic flame spraying.
In the invention, the metal needle can be subjected to sand blasting treatment to improve the surface roughness thereof so as to improve the adhesion of the coating, specifically, the surface of the metal needle can be firstly washed clean by clean water and subjected to sand blasting treatment until the surface roughness is more than 2.0 μm, then the surface of the metal needle is cleaned by absolute ethyl alcohol or acetone, and the wear-resistant coating is sprayed after the surface of the metal needle is cleaned. The sand blasting treatment may use white corundum, copper ore sand, quartz sand, silicon carbide, iron sand, sea sand, or the like.
Examples
Example 1
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
8.5kg of zirconium oxide fine particles (average particle size of 0.01 μm), 0.5kg of boron nitride fine particles (average particle size of 0.02 μm), 2kg of yttrium oxide (average particle size of 0.03 μm), 3kg of cerium oxide (average particle size of 0.02 μm), 2kg of titanium oxide (average particle size of 0.01 μm), and 3kg of tin oxide (average particle size of 0.05 μm) were mixed uniformly for use.
And spraying the mixed particles onto a metal needle by a plasma spraying method, wherein the spraying parameters comprise that the flow of main gas Ar is 60L/min, the flow of auxiliary gas H2 is 10L/min, the flow of powder feeding gas Ar is 6L/min, the powder feeding rate is 15g/min, the current is 500A, the gun swing speed is 600mm/s, the spraying distance is 70mm, the spraying angle is 90 ℃, and the mixed particles are cooled for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 1 mu m.
Example 2
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
8.7kg of zirconia fine particles (average particle size of 0.1 μm), 0.4kg of boron nitride fine particles (average particle size of 0.2 μm), 3kg of yttria (average particle size of 0.1 μm), 2kg of alumina (average particle size of 0.2 μm), 2kg of titania (average particle size of 0.3 μm), and 2kg of scandia (average particle size of 0.2 μm) were mixed uniformly for use.
And spraying the mixed particles onto a metal needle by a plasma spraying method, wherein the spraying parameters comprise that the flow of main gas Ar is 62L/min, the flow of auxiliary gas H2 is 11L/min, the flow of powder feeding gas Ar is 6L/min, the powder feeding rate is 16g/min, the current is 500A, the gun swing speed is 600mm/s, the spraying distance is 70mm, the spraying angle is 85 ℃, and the mixed particles are cooled for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 5 microns.
Example 3
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
9.0kg of zirconia fine particles (average particle size of 0.5 μm), 0.3kg of boron nitride fine particles (average particle size of 0.8 μm), 2kg of cerium oxide (average particle size of 0.6 μm), 2kg of titanium oxide (average particle size of 0.8 μm), and 3kg of silicon oxide (average particle size of 0.5 μm) were mixed uniformly for later use.
And spraying the mixed particles onto a metal needle by a plasma spraying method, wherein the spraying parameters comprise that the flow of main gas Ar is 63L/min, the flow of auxiliary gas H2 is 11L/min, the flow of powder feeding gas Ar is 6L/min, the powder feeding rate is 18g/min, the current is 500A, the gun swing speed is 600mm/s, the spraying distance is 70mm, the spraying angle is 80 ℃, and the mixed particles are cooled for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 10 mu m.
Example 4
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
9.2g of zirconia fine particles (average particle size of 1 μm), 0.1kg of boron nitride fine particles (average particle size of 1.5 μm), 2kg of strontium oxide (average particle size of 0.8 μm), 2kg of titanium oxide (average particle size of 1 μm), and 3kg of silicon oxide (average particle size of 1 μm) were mixed uniformly for use.
And spraying the mixed particles onto a metal needle by a plasma spraying method, wherein the spraying parameters comprise that the flow of main gas Ar is 65L/min, the flow of auxiliary gas H2 is 10L/min, the flow of powder feeding gas Ar is 6L/min, the powder feeding rate is 18g/min, the current is 600A, the gun swing speed is 550mm/s, the spraying distance is 65mm, the spraying angle is 80 ℃, and cooling is carried out for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 50 mu m.
Example 5
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
9.1kg of zirconia fine particles (average particle size 2 μm), 0.2kg of boron nitride fine particles (average particle size 1.8 μm), 2kg of cerium oxide (average particle size 2 μm), 2kg of alumina (average particle size 1.8 μm), and 3kg of silica (average particle size 2 μm) were mixed uniformly for use.
And spraying the mixed particles onto a metal needle by a plasma spraying method, wherein the spraying parameters comprise that the flow of main gas Ar is 65L/min, the flow of auxiliary gas H2 is 12L/min, the flow of powder feeding gas Ar is 6L/min, the powder feeding rate is 18g/min, the current is 550A, the gun swing speed is 550mm/s, the spraying distance is 65mm, the spraying angle is 85 ℃, and cooling is carried out for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 80 mu m.
Example 6
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
9.3kg of zirconia fine particles (average particle size of 3 μm), 0.05kg of boron nitride fine particles (average particle size of 3.5 μm), 2kg of cerium oxide (average particle size of 4 μm), 2kg of titanium oxide (average particle size of 3 μm), and 2.5kg of silicon oxide (average particle size of 3.8 μm) were mixed uniformly for use.
And spraying the mixed particles onto a metal needle by a plasma spraying method, wherein the spraying parameters comprise that the flow of main gas Ar is 65L/min, the flow of auxiliary gas H2 is 12L/min, the flow of powder feeding gas Ar is 6L/min, the powder feeding rate is 20g/min, the current is 550A, the gun swing speed is 500mm/s, the spraying distance is 60mm, the spraying angle is 80 ℃, and the mixed particles are cooled for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 100 mu m.
Example 7
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
9.5kg of zirconium oxide fine particles (average particle size 5 μm), 0.01kg of boron nitride fine particles (average particle size 5.2 μm), 2.3kg of cerium oxide (average particle size 5 μm), 1.6kg of titanium oxide (average particle size 4.9 μm), and 1kg of silicon oxide (average particle size 5 μm) were mixed uniformly for use.
And spraying the mixed particles onto a metal needle by a plasma spraying method, wherein the spraying parameters comprise that the flow of main gas Ar is 60L/min, the flow of auxiliary gas H2 is 10L/min, the flow of powder feeding gas Ar is 7L/min, the powder feeding rate is 20g/min, the current is 600A, the gun swing speed is 600mm/s, the spraying distance is 60mm, the spraying angle is 75 ℃, and the mixed particles are cooled for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 100 mu m.
Example 8
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
9.0kg of zirconia fine particles (average particle size of 0.5 μm), 0.3kg of boron nitride fine particles (average particle size of 0.8 μm), 2kg of cerium oxide (average particle size of 0.6 μm), 2kg of titanium oxide (average particle size of 0.8 μm), and 3kg of silicon oxide (average particle size of 0.5 μm) were mixed uniformly for later use.
Spraying the mixed particles onto a metal needle by a supersonic flame spraying method, wherein the spraying parameters comprise 80mL/min of propane, 200mL/min of oxygen and 20mL/min of nitrogen, the spraying distance is 60mm, the length of a spray pipe is 120mm, and cooling is carried out for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 10 microns.
Example 9
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
9.2g of zirconia fine particles (average particle size of 1 μm), 0.1kg of boron nitride fine particles (average particle size of 1.5 μm), 2kg of strontium oxide (average particle size of 0.8 μm), 2kg of titanium oxide (average particle size of 1 μm), and 3kg of silicon oxide (average particle size of 1 μm) were mixed uniformly for use.
Spraying the mixed particles onto a metal needle by a supersonic flame spraying method, wherein the spraying parameters comprise 85mL/min of propane, 300mL/min of oxygen and 50mL/min of nitrogen, the spraying distance is 65mm, the length of a spray pipe is 100mm, and cooling is carried out for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 50 microns.
Example 10
Manufacturing an abrasion-resistant coating on a metal needle of a polyimide film stretcher, cleaning the surface of the metal needle, specifically, washing the surface of the metal needle with clean water, performing sand blasting treatment on the surface of the metal needle with white corundum until the surface roughness is more than 2.0 mu m, and then cleaning the surface of the metal needle with absolute ethyl alcohol until the surface is crystallized for later use.
9.1kg of zirconia fine particles (average particle size 2 μm), 0.2kg of boron nitride fine particles (average particle size 1.8 μm), 2kg of cerium oxide (average particle size 2 μm), 2kg of alumina (average particle size 1.8 μm), and 3kg of silica (average particle size 2 μm) were mixed uniformly for use.
Spraying the mixed particles onto a metal needle by a supersonic flame spraying method, wherein the spraying parameters comprise 90mL/min of propane, 400mL/min of oxygen and 80mL/min of nitrogen, the spraying distance is 70mm, the length of a spray pipe is 120mm, and cooling is carried out for 48 hours at room temperature to obtain the wear-resistant coating with the thickness of 80 microns.
Test example
(1) Hardness test
The hardness of the coating is tested by a pencil scratch hardness tester according to GB/T6739-2006 Pencil method paint film hardness. During the test, the coating was placed on a horizontal surface and the coating was scratched at an angle of about 45 ° with pencils of different hardness (6H-6B), starting with the hardest 6H pencil, at a speed of 1mm/s with the aid of an auxiliary device, for 5 scratches of about 3mm length per step, until 5 pencils were found which did not scratch the coating, at which point the pencil hardness was representative of the coating hardness.
(2) Fracture toughness
The fracture toughness of the coating is measured by adopting an indentation method, the Vickers indentation method is prepared by adopting a Vickers hardness tester HV30 of Shanghai Shang material company, the loading load is 294.2N, the loading time is 15s, five points are selected for each sample to be measured, and the average value of the five points is taken. Fracture toughness KIC (MPa. m)1/2) Is calculated as follows:
p is applying load; HV: vickers hardness; c is half the crack length.
(3) Frictional wear performance
Carrying out a friction and wear test by adopting an HT-1000 type high-temperature friction and wear testing machine, wherein the test conditions are as follows: the test temperature is room temperature, the counter-grinding material is WC ceramic balls, the rotating speed is 560r/min, and the measured load is 10N. Before testing, the surface of the sample is polished by sand paper and leveled, and then is cleaned by absolute ethyl alcohol ultrasonic wave for 10min, and the sample is dried, and the abrasion weight loss is weighed by a BT224S type analytical balance with the precision of 0.0001 g.
(4) Coefficient of thermal expansion
The thermal expansion coefficient of the coating was measured using the us DIL802 equipment at a temperature ranging from room temperature to 1300 c and averaged.
| Hardness (H) | Fracture toughness (MPa. m)1/2) | Amount of wear (△ m/mg) | Coefficient of thermal expansion (. times.10)-6K-1) | |
| Example 1 | 6 | 6.5 | 0.55 | 10.6 |
| Example 2 | 6 | 6.8 | 0.59 | 10.5 |
| Example 3 | 6 | 7.1 | 0.45 | 10.6 |
| Example 4 | 6 | 7.3 | 0.48 | 10.2 |
| Example 5 | 6 | 7.2 | 0.42 | 10.8 |
| Example 6 | 6 | 6.9 | 0.50 | 10.5 |
| Example 7 | 6 | 6.5 | 0.52 | 10.6 |
| Example 8 | 6 | 7.0 | 0.46 | 10.5 |
| Example 9 | 6 | 7.1 | 0.48 | 10.2 |
| Example 10 | 6 | 6.8 | 0.51 | 10.1 |
As is clear from the above test examples, the coating of the present invention has high hardness, high fracture toughness, low embrittlement resistance, wear resistance, and a low thermal expansion coefficient at high temperatures.
Effect test
(1) Experimental examples of Effect
Pyromellitic dianhydride and 4, 4' -diaminodiphenyl ether in equal molar ratio are used as binary anhydride and diamine, N-dimethylformamide is used as a solvent, the viscosity is 40000-4.50000cps (20 ℃), and the imidization temperature is set to be 300-400 ℃. In which an abrasion-resistant coating was produced on the metal needle of a polyimide film stretcher as in example 4. After one month of continuous production, the obtained polyimide film was subjected to a performance test.
(2) Comparative example 1
The same effects as in the above-mentioned experimental examples were obtained except that the thickness of the coating layer on the metal needle of the polyimide film stretching machine was 150. mu.m.
(3) Comparative example 2
The same effects as those in the above-described experimental examples were obtained except that the coating according to the present invention was not sprayed on the metal needle of the polyimide film stretching machine.
From the above experiment, it can be seen that in comparative example 2 in which the coating according to the present invention was not applied to the metal needle of the polyimide film stretching machine, the metal needle was corroded and worn when polyimide was produced by a long-term operation, and metal chips after the wear fell and remained on the metal needle. Comparative example 1, the coating of the present invention was sprayed on the metal needle of the polyimide film stretching machine, but the spraying coating was too thick, which affected the stretching force of the polyimide film in the transverse direction and further affected the transverse tensile strength of the polyimide film. In the effect experiment example, the proper amount of the coating is sprayed, so that the mechanical property of the polyimide film is not influenced, the corrosive wear of the metal needle is effectively prevented, the durability of the metal needle is enhanced, and the polyimide film with clean appearance can be prepared.
Claims (10)
1. A wear-resistant coating for a polyimide film stretcher is characterized in that the coating contains 85-95% of zirconia.
2. The wear-resistant coating according to claim 1, wherein the coating further comprises 0.1 to 5% of boron nitride.
3. The wear-resistant coating according to claim 1 or 2, wherein the balance of the coating is one or more of yttrium oxide, silicon oxide, aluminum oxide, scandium oxide, cerium oxide, titanium oxide, tin oxide, strontium oxide.
4. The wear-resistant coating according to any one of claims 1 to 3, wherein the coating thickness is 1 to 100 μm.
5. The method for producing a wear-resistant coating according to any one of claims 1-4, characterized in that it comprises the following steps:
(1) cleaning the surface of the metal needle;
(2) drying the raw materials for the wear-resistant coating, uniformly mixing, and spraying the mixture on the surface of the metal needle;
(3) drying at room temperature.
6. The method of manufacturing of claim 5, wherein the spraying comprises any one of supersonic flame spraying, plasma spraying, cold spraying, electric arc spraying, and suspension spraying.
7. The manufacturing method according to claim 6, wherein the spraying is plasma spraying, and the spraying parameters are: the flow rate of main gas Ar is 60-65L/min, and the flow rate of auxiliary gas H2The flow rate is 10-12L/min, the flow rate of Ar of the powder feeding gas is 6-7L/min, the powder feeding rate is 15-20 g/min, the current is 500-600A, the gun swing speed is 500-600 mm/s, the spraying distance is 60-70 mm, and the spraying angle is 75-90 degrees.
8. The manufacturing method according to claim 6, wherein the spraying is supersonic flame spraying, the used fuel gas is propane, the combustion-supporting gas is oxygen, the powder feeding gas is nitrogen, and the gas flow rates are respectively as follows: 80-90 mL/min propane, 200-400 mL/min oxygen and 20-80 mL/min nitrogen, the spraying distance is 60-70 mm, and the length of the spray pipe is 80-120 mm.
9. The production method according to claim 5, wherein the raw material for the wear-resistant coating layer has an average particle diameter of 0.01 to 5 μm.
10. The manufacturing method according to claim 5, wherein the step (1) is specifically: the surface of the metal needle is washed clean by clean water, sand blasting is carried out until the surface roughness is more than 2.0 mu m, and then the surface of the metal needle is cleaned by absolute ethyl alcohol or acetone.
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