TWI753776B - A compound for forming a protective layer on metals and its manufacturing method - Google Patents

Abstract

The invention relates to a compound for forming a protective layer on metals and its manufacturing method. The compound is produced by mixing chlorite powder, sepiolite, silica powder, dispersant, surfactant, and base oil together in a colloid mill (a common equipment for blending sticky matters). Then, add the compound in a propotion of 0.01 to 0.2 wt.% into lubricating medium; a protective layer is going to form on the working metal friction part.

Description

A composition and preparation method are used for forming a protective layer on a metal surface.

The present invention relates to a composition and a preparation method for forming a protective layer on a metal surface, more particularly, to a composition and a preparation method for forming a protective layer on a metal friction surface

A large part of the high performance of precision equipment is the guarantee of ultra-high performance on the surface of metal friction parts. Modern metal surface technology can be divided into three categories: modification technology, thin film technology and coating technology. According to the surface formation principle, it can be subdivided into more than 20 kinds, such as chemical-electrochemical deposition, chemical conversion, surfacing, hot and cold spraying, adhesive technology, shot peening technology, chemical vapor deposition, ion implantation, electron beam cladding, laser remelting And so on, all are to change the type, chemical composition, organizational structure and stress state of the solid metal surface or non-metal surface to obtain the required surface properties to support the function of the device.

Furthermore, according to a large number of previous technical investigations and references, failure causes of metal parts and other documents, it can be seen that surface technology has great limitations and deficiencies. The details are as follows: (1) Some metal parts are complicated in structure and cannot be treated with the above surface technology; (2) Some metal parts have higher requirements on the heat-affected zone and cannot be treated with the above surface technology; (3) The above surface technologies are all realized The improvement or change of a certain surface property, with functional unity; (4) in the application of equipment for processing semiconductor components (5) The biggest shortcoming of current surface technology is offline pretreatment, which cannot be completed under the working state of equipment parts.

Among them, in the application of equipment for processing semiconductor components, a passivation layer, such as a polyamide layer, is often applied to the metal surface of the equipment, and several solder bump structures can be formed therein. For this purpose, process techniques that are recognized as effective for polyamide materials can be used to lay down the material and subsequently pattern it, followed by deposition of a conductive material, to provide a correlation with another material (eg, lead-free solder material and the like) appropriate interface features. As a result, if semiconductor device processing and solder bump structures to form polyamide materials are done at a remote fabrication site, degrading the copper surface can cause substantial yield loss unless extensive reworking is done; however, This may require additional tooling resources not normally available at any such manufacturing location. On the other hand, providing a dedicated final metal layer (eg, aluminum) or forming a solder bump structure in a fabrication facility that forms the metallization system may require additional resources that are often incompatible with the existing equipment and configurations of the semiconductor fabrication facility. That said, many additional resources may have to be provided.

The contents disclosed in the above background description paragraphs are only for enhancing understanding of the background of the present invention. Therefore, the above contents do not constitute prior art that hinders the present invention, and should be well known to those skilled in the art.

In order to make up for the above-mentioned deficiencies of the prior art, the present invention provides a method for forming a multiphase microcrystalline protective layer on a metal friction surface and a composition thereof. In the present invention, the composition of the present invention can be added in proportion to the lubricating medium used in the metal friction part, such as the most common grease, lubricating oil, and the use of the metal friction part to work without relying on special equipment and complicated processing technology. Under the state, running for 1-100 working hours, a 2-15 micron thick complex microcrystalline protective layer is formed on the metal friction part, and at the same time, the change and optimization of the metal surface morphology, chemical composition structure and stress state are realized. Further, the comprehensive performance of the surface of the metal friction part can be improved, and the industrialization promotion and large-scale production can be well realized.

Specifically, the present invention provides a method for preparing a composition, comprising: mixing 3-8 parts of chlorite powder, 8-18 parts of sepiolite, 2-5 parts of silica powder, 5- 8 parts of dispersant, 2-3 parts of surface modifier and 30-50 parts of base oil are mixed into a composition solution; the composition solution is put into a colloid mill for processing; and the processed product is taken out to obtain the combination.

In certain embodiments, the processing time in the colloid mill is 3 hours.

The present invention further provides a method for forming a protective layer on a metal surface, comprising: adding the above-mentioned composition to a lubricating medium to form a mixture with a weight ratio of 0.01-2wt%; applying the mixture to the metal surface in a working state; It is applied to the metal surface in the working state; and when the metal surface is in the working state, a protective layer is formed on the friction part of the metal surface.

In certain embodiments, the metal surface is in operation for 1 to 100 hours.

In some specific embodiments, the thickness of the protective layer is 2-15 microns.

The invention has the following advantages: (1) it can be completed in the working state of the metal friction parts, without the need to stop and disassemble, which saves time and effort, is extremely convenient to use, and is very suitable for large-scale promotion; (2) can change or optimize the metal friction at the same time. The morphology, chemical composition, structure and stress state of the surface can realize the multi-phase microcrystalline protective layer and also have a certain function of compensating the wear of the metal friction part; (3) the application of the present invention is almost not limited by the size and structure of the friction part parts , as long as the friction part is in the working state and lubricated with lubricating oil or grease, a complex phase microcrystalline protective layer can be formed on the friction surface; (4) the complex phase microcrystalline protective layer is realized by the present invention, and the surface roughness is lower than the original processing. , the smooth friction surface has obvious optimization effect on the fitting clearance, vibration and noise of friction parts; (5) the invention It is obvious that special equipment is not required when the treatment is carried out, the complex treatment process and the operation of very professional technical personnel are not required, and the processing cost is low.

The details of one or more embodiments of the invention are set forth in the accompanying drawings and the description below. The technical features, objects and advantages of the present invention will be readily understood from these descriptions and drawings and the scope of the claims. At the same time, in order to make the above-mentioned features and advantages of the present invention more obvious and easy to understand, the following embodiments are given and described in detail with the accompanying drawings.

Other features and effects of the present invention will be clearly presented in the embodiments with reference to the drawings, wherein: Figures 1A and 1B are optical microscopes (200 times) for analyzing a sample one cylinder with and without the use of the composition of the present invention, respectively. Figure 2A and 2B are FE-SEM (500 times) respectively for using and not using the composition of the present invention to analyze the side profile of a sample-cylinder liner; Figures 3A and 3B are FE-SEM ( 500 times) respectively with and without the use of the composition of the present invention to analyze the profile view of the line rail of the second sample; FIG. 4 is a schematic diagram illustrating the measurement position of the second embodiment of the present invention.

The advantages and features of the present invention and the methods for achieving the same will be better understood by being described in more detail with reference to the exemplary embodiments and the accompanying drawings. However, the present invention may be embodied in different forms and should not be construed as limited to the embodiments set forth herein. On the contrary, the relevant technical field has These embodiments are provided so that this disclosure will be thorough, thorough, and complete to convey the scope of the invention to those of ordinary skill, and the invention will only be defined by the appended claims.

Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be more understandable that terms such as those defined in commonly used dictionaries should be construed as having meanings consistent with the meanings in the relevant art, and should not be construed in an overly formal meaning unless explicitly defined herein.

The singular forms "a," "at least one," and "the" as used herein may also include plural referents unless the context clearly dictates otherwise. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

差之內，例如，該實際數值為在一特定數值或範圍的±10%、±5%、±1%、或±0.5%以內。 In this paper, the numerical values and parameters used to define the scope of the present invention inevitably contain standard deviations caused by individual test methods, so they are mostly expressed in approximate numerical values. However, in the specific embodiments, the Relevant numerical values presented as precisely as possible. As used herein, "about" generally depends on the considerations of those of ordinary skill in the art to which the present invention pertains, and generally refers to an acceptable standard representing an actual value falling within an average value

Within a difference, for example, the actual value is within ±10%, ±5%, ±1%, or ±0.5% of a particular value or range.

The present invention mainly provides a method for forming a protective layer on a metal friction surface and a composition thereof. The composition is mainly prepared by the following method: 3-8 parts of chlorite powder, 8-18 parts of sea foam are prepared by weight ratio. Stone, 2-5 parts of silica powder, 5-8 parts of dispersant, 2-3 parts of surface modifier and 30-50 parts of base oil are put into a colloid mill and processed for 3 hours. The special composition of the present invention is composed of chlorite powder, sepiolite powder, silica powder, auxiliary agent and base oil, wherein the above parts refer to parts by weight.

In addition, the present invention also provides a method for forming a protective layer on a metal surface: the composition of the present invention is added to the lubricating medium used in the metal friction part in a weight ratio of 0.01 to 2%, and under the working state of the metal friction part, The lubricating medium brings the special composition particles of the present invention into the friction surface of the friction part, and the high contact pressure generated by the particles of the composition on the friction surface of the metal friction part is combined with the extrusion and rolling generated by the relative movement between the metal friction surfaces. Under the repeated action of the force, a complex phase microcrystalline protective layer is formed on the friction surface, and has a certain compensation function for the surface of the metal friction part. The friction surface effectively forms a protective layer of complex microcrystalline.

The technical features of the present invention are not obvious because the technical features of the above judgment are all expressed in a "quantitative" way, and the defined numerical values are all in line with the judgment method, so they are all key numerical values, which are different from the general prior art. There are substantial and significant differences with outstanding substantive characteristics.

Illustrative embodiments are described below in conjunction with the detailed description. These embodiments, however, may be embodied in different forms and should not be construed as limiting the scope of the claims of the present invention. These embodiments are provided so that the disclosure of the present invention will be complete and clear, and those skilled in the art will be able to understand the scope of the present invention through these embodiments.

"Example 1"

The following examples illustrate the tested effects of the present invention, which are only illustrative, and are not intended to limit the scope of the present invention.

Sample 1: Cylinder liner metal block (ductile iron); Sample 2: Line rail (bearing steel) (brand: THK; model: LM Guide SHS35LC 4QZSSFM-5960LTF).

macroscopic analysis

Grind the test piece to No. 1500 sandpaper, use polishing liquid and polishing cloth to polish the surface to the mirror surface, and perform macroscopic analysis without corrosion.

Micro analysis

The samples 1 and 2 were ground and polished to the mirror surface by metallographic method, and the microscopic analysis was carried out by optical microscope (OM BX41M), high-resolution field emission scanning electron microscope (FE-SEM JSM-7900F), and magnification. And the difference in hardness was detected by a nano-indentation mechanical property analyzer (Hysitron TI980 TriboIndenter), as follows.

The first and second samples were subjected to surface treatment and block size treatment to capture the size of the FE-SEM size limit, and then use different analysis equipment to test the appearance, composition and hardness.

Macroscopic Analysis Results

After one side of the sample is ground and polished, there is no obvious deformation and crack in appearance, and there is rust on the front side and dents after wear. After the two sides of the sample are ground and polished, there is no obvious deformation and crack in appearance, and the concave part of the line rail is foggy, and there are reactants remaining.

Micro Analysis Results

The lateral morphology of the sample-cylinder liner was analyzed with and without the use of the composition of the present invention by an optical microscope, respectively, as shown in FIG. 1A and FIG. 1B , respectively.

Using FE-SEM to analyze the lateral morphology of the sample-cylinder liner with and without the use of the composition of the present invention, respectively, as shown in FIG. 2A and FIG. 2B .

The hardness test results of the surface of the sample one without using the composition of the present invention were tested by a nano-indentation mechanical property analyzer as shown in Table 1 below.

The average hardness of the cylinder liner without using the composition of the present invention = 7.68 GPa.

In contrast, the hardness test results of the surface of the sample using the composition of the present invention were measured by a nano-indentation mechanical property analyzer as shown in Table 2 below.

There is an average hardness of cylinder liner using the composition of the present invention = 10.30 GPa.

In addition, using FE-SEM to analyze the side surface of the line track of the second sample with and without the use of the composition of the present invention, as shown in FIG. 3A and FIG. 3B , respectively.

The hardness test results of the two surfaces of the two surfaces of the samples without using the composition of the present invention were tested by a nano-indentation mechanical property analyzer as shown in Table 3 below.

The mean value of rail hardness without using the composition of the present invention = 5.12 GPa.

In contrast, the hardness test results of the two surfaces of the two surfaces of the samples using the composition of the present invention were tested by a nano-indentation mechanical property analyzer as shown in Table 4 below.

There is an average value of rail hardness = 10.66 GPa using the composition of the present invention.

This example can be confirmed by sample 1 and sample 2. When a material using the composition of the present invention is coated on a metal friction surface, the surface has a higher hardness value.

"Example 2"

In this example, the slide rail, the slider and the ball screw are tested; among them, the slide rail model: EGR20R340P (precision grade; P grade), the slider model: EGH20SAZ0P (precision grade; P grade), the brand is Shanghai Silver Technology; Ball screw model: NSK-MCM05, the brand is NSK.

Test process: connect the ball screw with the linear slide rail and slider, the speed of the ball screw can be adjusted, the stroke is 150mm reciprocating movement, the maximum speed is 300mm/sec; (1) The actual working condition of the analog guide rail device: use the ball screw to operate the power to connect After connecting the ball screw, the guide rail and the slider, the device is installed on the test bench to form a set of analog slide rail operation test device; (2) Comparison scheme before and after the test - Linear slide rail: the reciprocating stroke of the ball screw is about 150mm long, and the linear slide rail is about 150mm long. The total length of the rail is 340mm, and the length of 150mm of the linear slideway is selected for the treatment test; (3) The new linear slideway raceway is tested by optical instruments without application and after the application of the composition of the present invention, the surface roughness of the raceway changes and 2D , 3D graphics.

Machine used: Line Guide Roughness measurement BMT Lab white light interferometer (BMT WLILab-300M; SANPANY), which is a non-contact 3D surface topography measurement and analysis system, non-destructive measurement, avoids damage to the sample surface, vertical resolution 0.1nm, the range is 0.1nm~10mm. Other parameters can be found in its product introduction, and will not be repeated here.

Please refer to Figure 4 for the description of the measurement position: (1) The raceways on both sides of the guide rail are divided into A and B raceways, the lower part of the front of the mark is the A raceway, and the upper part is the B raceway; (2) The guide rail has two unrepaired areas. Measuring point, A raceway: measuring point 1; B raceway: measuring point 2; (3) There are four side points in the repair range of guide rail repair materials, A raceway: measuring point 3, measuring point 5, B raceway: measuring Point 4, measuring point 6.

The following table 5 is the integration of the measurement data of the A raceway and the B raceway.

The linear slide rail and ball screw simulation treatment was carried out on the test bench with the composition of the present invention, and the test was accumulated for 1028 hours, and the following conclusions were drawn: (1) The composition of the present invention was used for comparison before and after use, and the new linear slide rail was rolled on the new linear slide rail. By applying the composition of the invention on the track, an ultra-hard and ultra-smooth metal-based composite nanocrystalline protective layer can be formed; (2) the formation range of the super-hard and smooth metal-based composite nanocrystalline protective layer of the linear track raceway, the surface structure of the raceway is dense, The gloss of the rail raceway is significantly higher than that before the application of the composition of the present invention Increase; (3) after 2 hours of operation by observation. The oil color is slightly black, indicating that the composition of the present invention has begun to work; (4) the effect of repair can be seen from the surface roughness measurement of 2D and 3D, and the surface roughness is obviously higher than that before the composition of the present invention is not applied. (5) Since the slider balls and ball slides are not easy to measure optically, it is observed with the naked eye. By reflective observation with the naked eye, it can be found that the ball slides produce fine line reflections at the friction place, similar to the linear rail slides. Therefore, it can be known that the composition of the present invention produces a superhard and supersmooth metal-based composite nanocrystalline protective layer on the surface of the ball and the ball slideway after friction, which can greatly increase the use time of the slider; (6) After comparison It can be found that the ball surface of the new slider is relatively rough. After the application of the composition of the invention, the superhard and supersmooth metal-based composite nanocrystalline protective layer on the surface of the slider ball is formed, the surface structure is dense, and the gloss of the ball is obviously improved compared with that before the application of the composition of the invention; (7) the sliding rail and the The surface roughness of the slider is greatly reduced under the action of the composition of the present invention, and the friction coefficient is relatively reduced. The sliding block runs more smoothly, so it can improve the vibration problem of the sliding rail operation and improve the precision of the sliding rail. In addition, the excellent wear resistance of the super-hard and slippery metal-based composite nanocrystalline protective layer can prolong the service life of the machine, reduce the maintenance cost of the machine and prolong the replacement cycle of the machine, which saves a lot of operating investment for the enterprise; Operational losses can be described as chronic diseases of machines, resulting in huge losses in business operations such as energy and machine downtime. The composition of the present invention can solve the above-mentioned problems at the bottom, and help owners save losses caused by machine wear.

To sum up, the composition of the present invention utilizes the heat energy generated by the friction of the mechanical equipment to dynamically complete the self-repair of the metal wear parts without the disintegration of the mechanical equipment, and generates a wear-resistant, super-hard and super-slippery metal matrix composite with excellent performance. Nanocrystalline protective layer has a wide range of applications, including but not limited to: various types of internal combustion engines, hydraulic systems, various types of compressors of different powers, various types of reducers, various types of bearings, open gear transmission devices, chain drives, Machine tool guide rails and other mechanical equipment with metal friction and wear.

All features disclosed in the present specification can be combined in any way. Features disclosed in this specification may be replaced by features of the same, equivalent or similar purpose. Accordingly, unless expressly stated otherwise, a feature disclosed in this specification is one embodiment of a series of equivalent or similar features.

In addition, according to the contents disclosed in this specification, those skilled in the art can easily make appropriate changes and modifications for different usage methods and situations according to the basic features of the present invention without departing from the spirit and scope of the present invention. Therefore, other Embodiments are also included in the scope of the patent application.

Claims (5)

A method for preparing a composition, comprising: mixing 3-8 parts of chlorite powder, 8-18 parts of sepiolite, 2-5 parts of silica powder, 5-8 parts of dispersant, 2-3 parts of Part of surface modifier and 30-50 parts of base oil are mixed into a composition solution; the composition solution is put into a two-colloid mill for processing; and one of the processed products is taken out to obtain the composition. The method according to claim 1, wherein the processing time in the colloid mill is 3 hours. A method for forming a protective layer on a metal surface, comprising: adding the composition of claim 1 to a lubricating medium used in a metal friction part in a weight ratio of 0.01 to 2% to form a mixture, and applying the mixture to a a metal surface in a working state; and a protective layer is formed on a friction part of the metal surface on the metal surface in the working state. The method as claimed in claim 3, wherein the metal surface is in the working state for 1 to 100 hours. The method according to claim 3, wherein the thickness of the protective layer is 2-15 microns.

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