CN112238392A - Centrifugal barrel polishing mechanical pre-polishing method for copper cavity substrate - Google Patents

Centrifugal barrel polishing mechanical pre-polishing method for copper cavity substrate Download PDF

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CN112238392A
CN112238392A CN202011054679.4A CN202011054679A CN112238392A CN 112238392 A CN112238392 A CN 112238392A CN 202011054679 A CN202011054679 A CN 202011054679A CN 112238392 A CN112238392 A CN 112238392A
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polishing
copper cavity
copper
cavity
abrasive
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CN112238392B (en
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杨馥羽
张沛
李中泉
戴劲
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Institute of High Energy Physics of CAS
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Institute of High Energy Physics of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B31/00Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor
    • B24B31/02Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor involving rotary barrels
    • B24B31/03Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor involving rotary barrels the workpieces being continuously-travelling
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The invention discloses a centrifugal barrel polishing mechanical pre-polishing method for a copper cavity substrate, which comprises the following steps of: 1) selecting a corundum oblique triangle as an abrasive, mixing the corundum oblique triangle with diluted grinding liquid, pouring the mixture into a copper cavity, and performing primary rolling polishing on the copper cavity substrate for 40-50 hours by adopting a centrifugal rolling polishing method; 2) selecting a resin cone as an abrasive, mixing the resin cone with diluted grinding liquid, pouring the mixture into a copper cavity, and performing secondary rolling polishing on the copper cavity substrate for 25-30 hours; 3) selecting bullet-shaped resin as an abrasive, mixing the bullet-shaped resin with diluted grinding liquid, pouring the mixture into a copper cavity, and performing third rolling polishing on the copper cavity substrate for 25-30 hours; 4) selecting corncobs as abrasive materials, mixing the corncobs with metal polishing paste, pouring the mixture into a copper cavity, and performing rolling polishing on the copper cavity substrate for the fourth time; the volume of the selected grinding material accounts for 38-42% of the total volume of the copper cavity each time, and the dosage of the metal polishing paste accounts for 1% of the volume of the corncob.

Description

Centrifugal barrel polishing mechanical pre-polishing method for copper cavity substrate
Technical Field
The invention relates to a centrifugal barrel polishing mechanical pre-polishing method, in particular to a centrifugal barrel polishing mechanical pre-polishing method for a copper cavity substrate plated with niobium through vacuum magnetron sputtering.
Background
The full name of accelerators is "charged particle accelerators," which are devices that artificially generate high-energy beams of charged particles. It uses a certain form of electromagnetic field to accelerate the charged particles such as electrons, protons, light and heavy ions, so that their speed can reach the level close to the speed of light. This kind of particle beam with relatively high energy is an important tool for people to change the atomic nucleus, study 'elementary particles' and know the deep structure of matter. The particle accelerator is a complex high-technology engineering device and mainly comprises four basic parts: the device comprises a particle source, a vacuum acceleration chamber, a guide focusing system and a beam transporting and analyzing system. The vacuum acceleration chamber is a vacuum chamber with an acceleration structure, and generates an acceleration electric field with a certain shape in vacuum, so that the particles are accelerated under the condition of not being scattered by air molecules, such as a high-frequency acceleration cavity. The high-frequency system is the heart of the accelerator, converts electric energy into microwave power, the microwave power is fed into the high-frequency cavity, and an electromagnetic field is excited in the microwave power and transmitted to charged particles, so that the charged particles are accelerated and supplemented with energy. At present, most of domestic high-frequency cavities are made of pure niobium superconducting materials, and the pure niobium superconducting cavities are developed for decades, the related technology is mature, and the gradient E is acceleratedaccAlready approaching the theoretical limit. Therefore, how to increase the acceleration gradient and reduce the running cost of the accelerator has been the research hotspot in the field of radio frequency superconduction. Among them, the research of niobium film superconducting cavity opens up another path for developing superconducting cavity. Regarding the manufacturing of the copper-niobium sputtering superconducting cavity, a superconducting niobium film is plated on a copper cavity substrate by adopting a magnetron sputtering method, so that the copper-niobium sputtering superconducting cavity is obtained. The whole coating process is carried out under high vacuum.
Since the 80 s of the 20 th century, the research on copper-niobium sputtering superconducting cavities has been started abroad, and the copper-niobium sputtering technology is applied to various frequencies and cavity types and is put into operation in accelerator large devices. In recent years, a copper substrate niobium-tin thin film superconducting cavity is also one of research hotspots in the thin film superconducting cavity. Therefore, for obtaining a thin film superconducting cavity with high radio frequency performance, the surface treatment of the copper substrate directly has important influence on the subsequent coating quality no matter the copper-niobium sputtering superconducting cavity or the copper substrate niobium-tin thin film is obtained.
According to research, the inner surface roughness of the copper cavity substrate directly influences the surface impedance of the superconducting cavity after film coating, and therefore the radio frequency performance of the superconducting cavity is directly influenced. The surface treatment of the copper cavity substrate internationally adopts mechanical polishing to remove macroscopic large defects, and then utilizes chemical polishing or electropolishing technology to etch an oxide layer, pollutants and microscopic projections of the copper cavity substrate, so that the inner surface of the copper cavity can achieve a mirror surface effect.
Since the 80 s of the 20 th century, the research on the niobium-plated superconducting cavity of the copper cavity has been started abroad, and in the aspect of the surface treatment of the copper cavity substrate, the research on chemical polishing (SUBU formula) and the research on electric polishing are carried out, and the two surface treatment technologies are successfully applied to the copper substrate of the film cavity. With respect to chemical polishing and mechanical pre-polishing before electropolishing, since the 90 s of the 20 th century, new mechanical polishing techniques were explored as a research focus in this field, aiming at replacing the conventional polishing method with new mechanical polishing pre-treatment techniques.
The research on the application of the Centrifugal barrel polishing technology (CBP) to the copper cavity substrate has been carried out in Japan KEK and the American JLAB laboratories, etc., and the technology utilizes the Centrifugal principle to realize the high-speed polishing treatment of workpieces in a grinding container barrel, which is divided into rotation and revolution motions with completely opposite directions. The centrifugal barrel polishing machine has a plurality of barrels, and can realize simultaneous polishing of a plurality of cavities. For soft metal material copper, the formula of the abrasive material suitable for the rolling polishing technology is the basis for determining the surface effect, and the surface effects obtained by different formulas can be greatly different. The JLAB laboratory discloses a centrifugal rolling and polishing formula for a copper cavity substrate in 2013, the formula is regarded as a standard formula commonly used internationally, and is divided into 4 steps, and the formula comprises the following specific steps:
step 1: beveling the ceramic block and grinding fluid, and performing roll polishing for: 20 hours;
step 2: resin cone and grinding fluid, and rolling polishing time: 17 hours;
and step 3: 3 μm diamond suspension + wood block, tumbling time: 30 hours;
and 4, step 4: 0.04 μm silica gel + wood block, tumbling time: for 90 hours.
According to JLAB research, the rough polishing of the first two steps of the formula can remove large defects in the copper cavity substrate and improve surface uniformity, but from the third step, because the wood block is introduced as a carrier of diamond suspension, the wood block and the diamond suspension are uniformly mixed and rolled for 30 hours, and visual observation and characterization analysis show that new scratches can be introduced into the surface morphology, so that the inner surface is roughened, and a JLAB laboratory also gives a question whether the wood block and the copper surface interact or not.
In addition, a comparative study was given according to the JLAB study, which found that diamond suspensions with a particle size of 3 μm in the third step gave better surfaces and fewer scratches than the 1 μ suspension. Therefore, the formula adopts the granularity of 3 mu m, but no detailed comparative study of other granularities is given, and before the invention, the application study of the JLAB formula is carried out, and the effect of the third step is found to be really unsatisfactory, so that the ideal pre-polishing effect cannot be obtained, and the subsequent chemical polishing is directly influenced, and the quality of vacuum coating is further influenced. Therefore, the repeatability is not high by adopting the formula.
The invention aims to solve the difficulty of mechanical polishing of a copper substrate for a thin film superconducting cavity (a copper substrate niobium film, a copper substrate niobium tri-tin film and the like), and the specific technical problems to be solved are as follows:
1) the problem that the traditional mechanical polishing can only reach the coarse grinding level of the copper cavity substrate with a complex cavity is solved, and the uniform polishing of the 1.3GHz ellipsoid copper cavity substrate is realized.
2) Realizing average roughness R of inner surface of copper cavityaClose to 0.1 μm, which facilitates subsequent chemical polishing or electropolishing.
3) Reduce the dependence and cost of this surface treatment technique to the manpower: because traditional mechanical polishing relies on manpower, if a new technology can be explored, the dependence on the manpower is weakened, and more machines are relied on, so that the labor cost is reduced, and the mass production of mechanical polishing of the copper cavity substrate can be realized.
Disclosure of Invention
Aiming at the technical defects, the invention establishes a set of formula and an implementation flow suitable for centrifugal rolling polishing of the copper cavity substrate, the technical scheme has high repeatability, can solve the problem of coarsening the inner surface of the copper cavity by a wood block, enables the inner wall of the copper cavity to achieve a mirror surface effect, can greatly reduce the labor cost, and greatly improves the automation degree of mechanical pre-polishing of the copper cavity substrate, thereby being beneficial to batch polishing of the copper cavity substrate in the future.
The technical scheme of the invention is as follows:
a centrifugal barrel polishing mechanical pre-polishing method for a copper cavity substrate comprises the following steps:
1) selecting a corundum oblique triangle as an abrasive, mixing the corundum oblique triangle abrasive with diluted grinding liquid, pouring the mixture into a copper cavity, performing first rolling polishing on the copper cavity substrate for 40-50 hours by adopting a centrifugal rolling polishing method, and then emptying the copper cavity; wherein the diluted grinding liquid is the grinding liquid and the deionized water with the volume ratio of 1%; the ratio of the volume of the currently selected grinding material to the total volume of the copper cavity is 38-42%; immersing the abrasive material in deionized water;
2) selecting a resin cone as an abrasive, mixing the resin cone abrasive with the diluted grinding liquid, pouring the mixture into a copper cavity, performing secondary rolling polishing on the copper cavity substrate for 25-30 hours by adopting a centrifugal rolling polishing method, and then emptying the copper cavity; the ratio of the volume of the currently selected grinding material to the total volume of the copper cavity is 38-42%; immersing the abrasive material in deionized water;
3) selecting bullet-shaped resin as an abrasive, mixing the bullet-shaped resin abrasive with the diluted grinding liquid, pouring the mixture into a copper cavity, performing rolling polishing on the copper cavity substrate for the third time for 25-30 hours by adopting a centrifugal rolling polishing method, and then emptying the copper cavity; the ratio of the volume of the currently selected grinding material to the total volume of the copper cavity is 38-42%; immersing the abrasive material in deionized water;
4) selecting corncobs as grinding materials, mixing the corncob grinding materials with metal polishing paste, pouring the mixture into a copper cavity, performing fourth rolling polishing on the copper cavity substrate by adopting a centrifugal rolling polishing method, and then emptying the copper cavity; the ratio of the volume of the currently selected grinding material (corncob) to the total volume of the copper cavity is 38-42%; the dosage of the metal polishing paste is 1 percent of the volume of the corncob.
Furthermore, the temperature of the copper cavity is controlled within 35 ℃ in the rolling and polishing process, and the temperature of the cavity wall of the copper cavity is maintained within 4 ℃ relative to the temperature rise before rolling and polishing.
Further, a 240-mesh corundum oblique triangle is selected as an abrasive; the resin cone is a 1000-mesh resin cone; the bullet-shaped resin is 2000-mesh bullet-shaped resin.
Further, the first rolling polishing time is 50 hours, and the roughness of the inner surface of the copper cavity reaches 0.315 mu m; the second rolling polishing time is 25 hours, and the roughness of the inner surface of the copper cavity reaches 0.283 mu m; the third rolling polishing time is 25 hours, and the average roughness of the inner surface of the copper cavity reaches 94 nm; the fourth polishing time is controlled to be 5-8 hours, and the roughness of the inner surface of the copper cavity reaches 61 nm.
Further, the optimal proportion of the abrasive volume to the total capacity of the copper cavity is 40%.
Further, the polishing solution is an alkaline polishing solution.
Further, ultrasonically degreasing the copper cavity treated in the step 4), cleaning by using deionized water, and blow-drying by using nitrogen.
Compared with the prior art, the invention has the following positive effects:
the invention successfully explores a formula and an implementation method suitable for copper cavity centrifugal rolling polishing, and the specific process is executed according to the attached figure 6. The method has high repeatability, promotes the automation of mechanical pre-polishing of the copper cavity, greatly reduces the dependence on manpower, and is beneficial to subsequent batch operation.
Drawings
FIG. 1 is a schematic diagram of centrifugal tumbling;
FIG. 2 is a view of the structure of the abrasive;
(a) a corundum oblique triangular structure of 240 meshes, (b) a conical structure of a resin material, (c) a bullet structure of the resin material;
FIG. 3 is a graph showing the effect of using resin cone abrasives for the amount of abrasives;
FIG. 4 is a temperature monitoring diagram of the centrifugal tumbling in winter and summer;
FIG. 5 is a surface evaluation chart of each step;
FIG. 6 is a flow chart of the centrifugal tumbling of the copper chamber substrate.
Detailed Description
The present invention is described in further detail below with reference to the attached drawings.
The invention aims to explore a set of centrifugal barrel polishing formula applied to the copper cavity substrate, so that the subsequent chemical polishing or electropolishing is facilitated, and the vacuum coating is carried out. The principle diagram of centrifugal roll polishing is shown in attached figure 1, and comprises a 1.3GHz ellipsoidal copper cavity substrate to be polished, and the rotation direction and the revolution direction in the centrifugal roll polishing are completely opposite. Under the combined action of rotation and revolution, the centrifugal force borne by the abrasive is vertical to the cavity wall (normal direction), and the abrasive and the cavity wall generate relative motion in the tangential direction, so that the polishing effect on the cavity wall is generated. The abrasive material is selected, the amount, the time, the temperature and other factors directly determine the polishing effect of the abrasive material on the cavity wall, so that the successful polishing on the centrifugal rolling polishing machine greatly depends on the selection of the formula. The invention discloses a formula suitable for centrifugal rolling polishing of a copper cavity substrate, and the specific technical scheme is as follows.
1. Selection of abrasive and grinding fluid
The copper cavity substrate needs to be uniformly polished from rough polishing to fine polishing and then to ultra-fine polishing, and proper grinding materials need to be selected in each stage. In the rough polishing stage, aiming at removing a mechanical damage layer with larger thickness from the copper cavity substrate, the requirement on the abrasive is high enough cutting capability, the invention selects the corundum oblique triangle on the market as the abrasive in the first step, and because each part is primarily polished before the copper cavity is welded and formed, the inner surface of the copper cavity after being formed does not need to be polished by a rough roll, thus the corundum oblique triangle with 240 meshes (granularity: 58.5 μm) is selected, and the specific shape is shown in figure 2 (a). After the corundum inclined triangle is rolled and polished for a certain time, the mechanical damage layer introduced by processing on the inner surface of the copper cavity is basically removed, but the uniformity of the inner surface is to be improved, and an abrasive needs to be selected to obtain the uniform inner surface. For copper metal, care is taken to select an abrasive that is too hard (possibly introducing pit morphology), and resin is an environmentally friendly and softer material, better suited for copper metal. Through the polishing of the first two steps, the copper cavity can obtain a more uniform inner surface, but the irregular scratches still exist. In the third step, a bullet-shaped resin material was used, as shown in FIG. 2(c), 2000 mesh (particle size: 10.3 μm) was selected. The 2000-mesh bullet type resin selected by the invention belongs to a fine abrasive customized by a manufacturer, wherein 2000-mesh fine sand grains are arranged inside the abrasive, the outside of the abrasive is wrapped by cured resin, the outer surface of the customized bullet type resin is rough, in order to avoid the influence of the outer surface of the abrasive on the inside of a copper cavity, the abrasive needs to be put into other sealed workpieces in advance, rolling and polishing are carried out for a certain time, the rough part of the surface is removed, the fine sand grains inside are exposed and then put into a copper cavity substrate to carry out the third step of rolling and polishing, and the scratches on the inner surface of the copper cavity are basically removed in a disordered way through the third step of polishing. And the hyperfine polishing of the fourth step adopts the combination of corncobs and metal polishing paste, and the corncobs are fine particles and have no definite shape. The two are evenly mixed and poured into a copper cavity, and are rolled and polished for a certain time, and experiments show that the inner surface of the copper cavity achieves the mirror effect. The above is the selection of the abrasive in the four steps of tumbling.
The grinding materials are solid, and under the high-speed rotation and revolution of the machine, if only the grinding materials are adopted, the friction between the grinding materials and the cavity wall can generate a large amount of heat, so that the inner surface of the copper oxide cavity is oxidized, and the grinding materials are matched with a proper amount of deionized water, and meanwhile, a proper grinding liquid is selected for preventing the grinding materials from being adhered to the cavity wall. The invention selects the alkaline grinding fluid, and the content of the alkaline grinding fluid is diluted according to the proportion of 1% (the dilution proportion is the volume ratio of the grinding fluid to the deionized water). The metal polishing paste is used in an amount of 1% by volume of the corncob.
Therefore, the abrasive of the invention is matched as follows: the first step is as follows: corundum oblique triangle (240 meshes), deionized water and alkaline grinding fluid (diluted by 1 percent); the second step is that: resin cone (1000 mesh), deionized water and alkaline grinding fluid (1% dilution); the third step: bullet type resin (2000 mesh) + deionized water + alkaline grinding fluid (1% dilution); the fourth step: corncob + metal polishing paste (1%).
2. Determination of the amount of abrasive
The dosage of the grinding material is a factor influencing centrifugal rolling polishing, a 1.3GHz copper cavity is a rotationally symmetrical cavity type, and under the rotation and revolution in a rolling polishing machine, the grinding material is too little, and the grinding material is concentrated in the area with the largest radius, namely the equatorial area of the copper cavity, so that other parts cannot be completely polished. If the abrasive is too much, the abrasive is more likely to stick on the cavity wall, and the polishing effect is affected. Therefore, the invention obtains the optimal abrasive material dosage through experimental comparison. As shown in FIG. 3, the abscissa represents the ratio of the volume of abrasive to the total volume of the copper cavity, the primary ordinate indicates the removal thickness, and the secondary ordinate represents the polishing rate. According to the invention, resin cone abrasives are adopted for researching the abrasive amount, deionized water required to be added in the rolling and polishing process is only required to ensure that the abrasives are basically submerged, the grinding liquid is diluted according to the proportion of 1% (the volume ratio of the grinding liquid to the deionized water is 1%), and researches show that the polishing rate obtained by 30% of abrasives is the lowest, after the proportion is increased to 40%, the polishing rate obtains the maximum value, the polishing rate is continuously increased to 50% and 60%, and the polishing rate is continuously reduced, so that the removal thickness and the polishing rate under the optimal abrasive amount are respectively represented as shown in figure 3. Experiments show that the ratio of the volume of the grinding material to the total volume of the copper cavity is lower than 40%, and the excessive consumption can not fully polish all parts of the copper cavity; the ratio of the volume of the grinding material to the total volume of the copper cavity is higher than 40%, and excessive use amount can cause the adhesion of the grinding material and the cavity wall and is not beneficial to improving the polishing efficiency. Therefore, the invention determines that the using amount of the grinding material can be 38-42%, the optimal using amount is 40%, namely the optimal proportion of the grinding material volume in the copper cavity volume is 40%. Similarly, in the fine polishing process of the fourth step, the optimal proportion of the volume of the corncobs in the volume of the copper cavity is also 40%, and the dosage of the metal polishing paste is 1% of the volume of the corncobs.
3. Temperature monitoring in tumble polishing
Although the addition of water during the tumbling process can reduce heat generation to some extent, the process must be strictly temperature monitored in order to prevent oxidation of the copper cavity due to heat during the tumbling. Because the environment temperature of the centrifugal rolling and polishing operation is different, the temperature of the outer surface of the cavity wall is different, the temperature monitoring is carried out in winter and summer, and the result is shown in figure 4. The temperature within 50 hours of the tumbling was monitored, with black dots representing temperature changes in summer and black triangles representing temperature changes in winter. The rolling and polishing machine is located at the room temperature of about 31 ℃ in summer and at the room temperature of about 14 ℃ in winter. By temperature monitoring, in the tumbling process, whether in winter or summer, the temperature rise of the cavity wall relative to the temperature rise of the cavity wall before tumbling is basically maintained within 4 ℃, the temperature rise is within a controllable range, and the highest temperature which can be reached by the cavity wall in the tumbling process in summer is within 35 ℃, and the temperature shows that no obvious heat is generated in the copper cavity tumbling process, so that additional cooling is not needed.
4. Copper cavity inner surface analysis
The average roughness of the inner surface of the copper cavity after rolling and polishing is a physical quantity which directly reflects the centrifugal rolling and polishing effect of the formula, the invention carries out surface evaluation on the inner surface of the formula after running in each step, the surface roughness measurement adopts a TR200 roughness meter, and the optical appearance is observed by adopting a portable Dino-Lite digital microscope. The results are shown in FIG. 5, respectively. The position of the number a in the attached figure 5 indicates the average roughness of the inner surface of the copper cavity before the barrel polishing treatment, and the average roughness is 0.317 μm, and the machining trace of the copper cavity in the inner surface optical topography of the copper cavity before the barrel polishing is obvious. After the corundum inclined triangle roll polishing in the first step is adopted for 25 hours, scratches and patterns on the inner surface of the copper cavity are obvious, so that the polishing time still needs to be prolonged, the position b in the figure 5, which is the number b, represents the roughness of the inner surface after 50 hours of corundum inclined triangle roll polishing in the first step of the formula, is 0.315 mu m, and the machining traces of the copper cavity are basically removed through the shape of the inner surface after 50 hours of corundum inclined triangle roll polishing, so that a 150 mu m damage layer is removed. Therefore, the rolling and polishing time of the corundum inclined triangle in the first step is about 40-50 h. The position of the number c in the attached figure 5 shows that the roughness of the inner surface after 25 hours of the second 1000-mesh resin cone is 0.283 mu m, the roughness is greatly improved, 90 mu m of the resin cone is removed by rolling and polishing, and the scratches are reduced. If the polishing time of the process is less than 25 hours, the roughness is not improved much, about 0.3 μm, and it is desired to obtain a more uniform inner surface, the barrel polishing time of the second step should be greater than or equal to 25 hours, i.e., the longer the barrel polishing time, the more remarkable the improvement. However, the grinding material size is reduced and the service life is reduced due to the overlong time, so that the rolling and polishing time of 25-30 h has the best effect. The position d of the reference number in the attached figure 5 shows the average roughness after 25 hours of rolling polishing of the third 2000-mesh resin cone, the average roughness is 94nm, and the rolling polishing removal amount is only about 4 mu m, which indicates that the thinner the abrasive, the smoother the inner surface of the copper cavity, the less the removal amount, and the scratches with disordered surface topography are basically polished and removed. In the rolling polishing of 10 hours, 15 hours and 20 hours, the scratches on the inner surface of the copper cavity which can be seen by naked eyes cannot be completely removed, the rolling polishing time is increased to 25 hours, the scratches on the inner surface of the copper cavity are basically removed, and the surface is smooth. And increasing the rolling polishing time, wherein the rolling polishing time exceeds 30 hours, the improvement of the inner surface of the copper cavity is not obvious, and the more the 2000-mesh abrasive is ground, the smoother the abrasive is, the lower the removal amount of the abrasive is, and the improvement effect basically does not exist afterwards. Therefore, the suitable range of the rolling polishing time of the third step is 25-30 h. The position of the number e in the attached figure 5 indicates the surface roughness after 5 hours of rolling polishing of the corncobs and the metal polishing paste, the surface roughness reaches 61nm, the removal amount is about 3 mu m, and the inner surface of the copper cavity generates a mirror surface effect. The step is less than 5 hours, the mirror effect of the inner surface of the copper cavity is not obvious, the proper rolling and polishing time is 5-8 hours, the time is too long, and the inner surface cannot be improved more obviously. In summary, the copper cavity substrate roll polishing formula applied in the invention can realize high-precision polishing and achieve mirror surface effect.
In summary, the specific implementation scheme of the present invention is:
1. determining the abrasive selection for each step: firstly, selecting 240-mesh corundum inclined triangle, deionized water and alkaline grinding fluid (1%); secondly, selecting 1000-mesh resin cone, deionized water and alkaline grinding fluid (1%); thirdly, determining 2000-mesh bullet-shaped resin, deionized water and alkaline grinding fluid (1%); the fourth step is to use corncob and metal polishing paste (1%).
2. Determining the usage ratio of the abrasive: the optimal proportion of the volume of the grinding materials in the total volume of the copper cavity is determined to be 40%, similarly, the optimal proportion of the volume of the corncobs selected in the rolling and polishing process of the fourth step in the total volume of the copper cavity is also 40%, and each process of the rolling and polishing of the copper cavity substrate is filled according to the optimal proportion. Wherein, the dosage of the deionized water is ensured to basically submerge the abrasive, and the dosage of the metal polishing paste is 1 percent of the volume of the corncob.
3. Determining the tumbling time: according to the inner surface condition of the 1.3GHz copper cavity substrate, the first-step rolling polishing time can be controlled to be about 40-50 hours, and the removal amount of enough thickness is ensured; the second step of rolling and polishing is controlled to be about 25-30 hours, so that uniform grinding is ensured; thirdly, controlling the rolling polishing time to be 25-30 hours to ensure that the surface roughness is reduced and scratches are completely removed; and fourthly, controlling the polishing time to be about 5-8 hours to ensure that the surface achieves the mirror effect. The rolling polishing time is too long, the service life of the grinding material is reduced, and the polishing efficiency is not high; the time is too short, and the inner surface condition is not improved too much.
4. Monitoring the temperature: through temperature monitoring in the rolling and polishing process, the temperature rise of the outer wall of the copper cavity in the rolling and polishing process is controlled within the range of 4 ℃ no matter the rolling and polishing operation is in winter or summer, the temperature rise belongs to an acceptable range, the rolling and polishing effect cannot be influenced, and cooling is not needed. In the rolling and polishing process, if the temperature of the copper cavity can be controlled within 35 ℃, the temperature can be considered to be controllable, and extra cooling operation is not needed.
5. Analysis of the internal surface: through the inner surface analysis of each step, the average roughness and the microscopic surface morphology are measured, and finally the formula is determined to be from rough polishing to ultra-fine polishing, the average roughness is reduced from 0.3 mu m to 60nm, and the inner surface of the copper cavity achieves the mirror surface effect.
In summary, the above are only some embodiments of the present invention, and are not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A centrifugal barrel polishing mechanical pre-polishing method for a copper cavity substrate comprises the following steps:
1) selecting a corundum oblique triangle as an abrasive, mixing the corundum oblique triangle abrasive with diluted grinding liquid, pouring the mixture into a copper cavity, performing first rolling polishing on the copper cavity substrate for 40-50 hours by adopting a centrifugal rolling polishing method, and then emptying the copper cavity; wherein the diluted grinding liquid is the grinding liquid and the deionized water with the volume ratio of 1%; the ratio of the volume of the currently selected grinding material to the total volume of the copper cavity is 38-42%;
2) selecting a resin cone as an abrasive, mixing the resin cone abrasive with the diluted grinding liquid, pouring the mixture into a copper cavity, performing secondary rolling polishing on the copper cavity substrate for 25-30 hours by adopting a centrifugal rolling polishing method, and then emptying the copper cavity; the ratio of the volume of the currently selected grinding material to the total volume of the copper cavity is 38-42%;
3) selecting bullet-shaped resin as an abrasive, mixing the bullet-shaped resin abrasive with the diluted grinding liquid, pouring the mixture into a copper cavity, performing rolling polishing on the copper cavity substrate for the third time for 25-30 hours by adopting a centrifugal rolling polishing method, and then emptying the copper cavity; the ratio of the volume of the currently selected grinding material to the total volume of the copper cavity is 38-42%;
4) selecting corncobs as grinding materials, mixing the corncob grinding materials with metal polishing paste, pouring the mixture into a copper cavity, performing fourth rolling polishing on the copper cavity substrate by adopting a centrifugal rolling polishing method, and then emptying the copper cavity; the volume of the currently selected corncob accounts for 38-42% of the total volume of the copper cavity, and the dosage of the metal polishing paste accounts for 1% of the volume of the corncob.
2. The method of claim 1, wherein the temperature of the copper chamber during barrel polishing is controlled to within 35 ℃ and the temperature of the walls of the copper chamber is maintained within 4 ℃ relative to the temperature rise prior to barrel polishing.
3. The method according to claim 1 or 2, characterized in that 240-mesh corundum scalene triangles are selected as the abrasive; the resin cone is a 1000-mesh resin cone; the bullet-shaped resin is 2000-mesh bullet-shaped resin.
4. The method of claim 3, wherein the first barrel polishing time is 50 hours and the roughness of the inner surface of the copper cavity reaches 0.315 μm; the second rolling polishing time is 25 hours, and the roughness of the inner surface of the copper cavity reaches 0.283 mu m; the third rolling polishing time is 25 hours, and the average roughness of the inner surface of the copper cavity reaches 94 nm; the fourth polishing time is controlled to be 5-8 hours, and the roughness of the inner surface of the copper cavity reaches 61 nm.
5. The method of claim 1, wherein the optimal proportion of abrasive volume to total volume of the copper chamber is 40%.
6. The method of claim 1, wherein the polishing slurry is an alkaline polishing slurry.
7. The method of claim 1, wherein the copper cavity treated in step 4) is ultrasonically degreased, then cleaned with deionized water, and then blown dry with high purity nitrogen.
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CN113385894A (en) * 2021-06-10 2021-09-14 中国科学院近代物理研究所 Radio frequency superconducting resonant cavity based on high-thermal-conductivity material and high-radio-frequency-performance superconducting material composite board and preparation method thereof
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