CN111331527B - Ultra-high porosity ceramic bond diamond ultra-precision grinding tool and preparation method thereof - Google Patents
Ultra-high porosity ceramic bond diamond ultra-precision grinding tool and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
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- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
- B24D3/04—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic
- B24D3/14—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic ceramic, i.e. vitrified bondings
- B24D3/18—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially inorganic ceramic, i.e. vitrified bondings for porous or cellular structure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
- B24D18/009—Tools not otherwise provided for
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
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- B24D3/346—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents characterised by additives enhancing special physical properties, e.g. wear resistance, electric conductivity, self-cleaning properties utilised during polishing, or grinding operation
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Abstract
The invention provides an ultra-high porosity ceramic bond diamond ultra-precision grinding tool and a preparation method thereof, relating to the technical field of ultra-precision grinding tools. The preparation method comprises the steps of mixing an amide organic monomer, a cross-linking agent and water to obtain a premixed aqueous solution; then sequentially adding mixed powder of the superfine diamond and the ceramic bond and a dispersing agent into the premixed water solution to obtain suspension slurry; adjusting the pH value of the suspension slurry to 9-11, and then carrying out ball milling; then adding a surfactant into the ball-milling slurry, and stirring the obtained slurry at a high speed to obtain a wet foam; adding a catalyst and an initiator into the wet foam, and carrying out gel curing on the obtained mixture in a mould; and (3) drying and sintering the porous blank obtained after demoulding in sequence to obtain the ultra-high porosity ceramic bond diamond ultra-precision grinding tool. The method provided by the invention can realize the uniform distribution of the ultra-fine diamond and the air holes in the grinding tool, and the air hole rate in the manufactured grinding tool is up to more than 75%.
Description
Technical Field
The invention relates to the technical field of ultra-precision grinding tool processing, in particular to an ultra-high porosity ceramic bond diamond ultra-precision grinding tool and a preparation method thereof.
Background
With the rapid development of industries such as optics, automobiles, communication industry, medicine, life science and the like, higher requirements are put forward on the surface processing quality and the processing efficiency of parts required by various industries; however, the surface roughness of the part processed by the existing common grinding processing technology is still between 0.16 and 1.25 μm, and the requirement of higher processing precision cannot be met. The ceramic bond ultra-precision grinding tool prepared by using the ultra-fine diamond has excellent characteristics of ultra-fine micro-blades, lower grinding stress and the like, can remove hard and brittle materials in a ductile grinding mode, can reduce subsurface damage and can obtain a high-quality machined surface.
However, most of the existing ceramic bond diamond ultra-precision grinding tools are prepared by the traditional cold pressing process and other methods, and ultra-fine diamond particles are unevenly dispersed in the structure of the grinding tool, so that the stability of the quality of the processed surface is uneven. Meanwhile, the porosity of the ultra-precision grinding tool prepared by the traditional forming process is generally less than 50%, and the pores are not uniformly distributed, so that not only can good cooling be realized, but also diamonds in the grinding tool are easily oxidized due to overhigh grinding temperature; and a large amount of fragments generated in the grinding process cannot be accommodated, so that pores of the grinding tool are easy to block, and the grinding performance of the ceramic bond diamond ultra-precision grinding tool is reduced.
Disclosure of Invention
In view of the above, the invention aims to provide an ultra-fine diamond grinding tool with an ultra-high porosity ceramic bond and a preparation method thereof. The method provided by the invention can realize uniform distribution of ultra-fine diamonds and pores in the grinding tool, can enable the porosity in the grinding tool to reach more than 75%, and obviously improves the grinding performance of the ceramic bond diamond ultra-precision grinding tool.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of an ultra-fine grinding tool of diamond with an ultra-high porosity ceramic bond, which comprises the following steps:
(1) mixing an amide organic monomer, a cross-linking agent and water to obtain a premixed aqueous solution;
(2) sequentially adding mixed powder and a dispersing agent into the premixed water solution to obtain suspension slurry; the mixed powder comprises ultra-fine diamond and a ceramic bonding agent;
(3) adjusting the pH value of the suspension slurry to 9-11, and then carrying out ball milling to obtain ball milling slurry;
(4) adding a surfactant into the ball-milling slurry, and then stirring and foaming the obtained slurry at a high speed to obtain a wet foam; the high-speed stirring speed is 1000-4000 r/min, and the time is 1-30 min;
(5) adding a catalyst and an initiator into the wet foam, carrying out gel curing on the obtained mixed foam in a mould, covering an organic solvent on the surface of the mixed foam, and demoulding to obtain a porous blank;
(6) and drying and sintering the porous blank in sequence to obtain the ultra-high porosity ceramic bond diamond ultra-precision grinding tool.
Preferably, the amide organic monomer in step (1) is acrylamide or N-vinyl pyrrolidone; the cross-linking agent is N, N' -methylene bisacrylamide or polyethylene glycol dimethacrylate; the mass ratio of the amide organic monomer to the cross-linking agent is 1-6: 1.
preferably, the mass concentration of the amide organic monomer in the premixed aqueous solution in the step (1) is 1-20%.
Preferably, the particle size of the superfine diamond in the mixed powder in the step (2) is less than or equal to 20 microns, and the particle size of the ceramic bond is 0.5-10 microns; the mass ratio of the superfine diamond to the ceramic bond is 10-50: 90-50; the mass of the mixed powder is 20-60% of that of the premixed water solution.
Preferably, the dispersant of step (2) comprises one or more of polyacrylic acid, ammonium polymethacrylate, ammonium citrate, tetramethylammonium hydroxide, sodium polyphosphate and ammonium polyacrylate; the mass of the dispersing agent is 1-18% of the mass of the mixed powder.
Preferably, the step (4) further comprises degassing the ball milling slurry before adding the surfactant; the degassing treatment method comprises the following steps: the ball-milled slurry was filtered and then stirred under vacuum.
Preferably, the surfactant in step (4) comprises one or more of Triton X-114, Tween80, sodium linear alkylbenzene sulfonate, sodium fatty alcohol-polyoxyethylene ether sulfate, ammonium fatty alcohol-polyoxyethylene ether sulfate, sodium lauryl sulfate, lauroyl glutamic acid, polyoxyethylene nonyl phenyl ether, peregal O, diethanolamide, glyceryl monostearate, lignosulfonate, heavy alkylbenzene sulfonate, alkyl sulfonate, NNO serving as a dispersing agent, MF serving as a dispersing agent, PO-EO copolymer and fatty alcohol-polyoxyethylene ether; the addition amount of the surfactant in each liter of ball milling slurry is 4-18 g.
Preferably, the catalyst in step (5) is N, N' -tetramethylethylenediamine; the initiator is ammonium persulfate; the catalyst is added in an amount of less than or equal to 7.5mL per liter of ball-milling slurry; the mass of the initiator is 0.2-3% of that of the ball-milling slurry.
Preferably, the drying in the step (6) comprises room temperature drying and heating drying which are sequentially carried out; the drying time at room temperature is 6-12 h; the heating and drying temperature is 60-100 ℃, and the time is 12-24 hours; the sintering temperature is 450-650 ℃, and the heat preservation time is 0.5-1 h.
The invention provides an ultra-high porosity ceramic bond diamond ultra-precision grinding tool prepared by the preparation method in the scheme, wherein the porosity of the grinding tool is more than or equal to 75%, and the size of pores is 100-350 μm.
The invention provides a method for preparing an ultra-fine grinding tool of ultra-high porosity ceramic bond diamond, which adopts a casting and condensing forming process and combines high-speed stirring foaming to prepare the ultra-fine grinding tool of ultra-high porosity ceramic bond diamond, in particular, air is introduced into slurry by high-speed stirring, forming a large amount of bubbles under the synergistic action of the surfactant, combining the polymerization reaction of the organic monomer with the molding of the superfine diamond and the ceramic bond powder in the process of gel curing, wherein the polymerization reaction of the organic monomer uniformly fixes the superfine diamond and the ceramic bond powder in situ in the polymer gel, the ultrafine diamonds can be uniformly distributed, a three-dimensional network structure formed by the ultrafine diamonds, the ceramic bond powder and the organic monomer is solidified into a bubble wall, and a blank contains a large amount of bubbles with uniform size; after the organic matter is oxidized and lost through sintering, the ceramic bond and the diamond fine particles are distributed on the wall of the air bubble. The method provided by the invention can realize uniform distribution of ultra-fine diamonds and pores in the grinding tool, can enable the porosity in the grinding tool to reach more than 75%, and obviously improves the grinding performance of the ceramic bond diamond ultra-precision grinding tool.
Drawings
FIG. 1 is a microscopic topography of the fracture of the sample of the ceramic bond diamond ultra-precision grinding tool prepared in example 2.
Detailed Description
The invention provides a preparation method of an ultra-fine grinding tool of diamond with an ultra-high porosity ceramic bond, which comprises the following steps:
(1) mixing an amide organic monomer, a cross-linking agent and water to obtain a premixed aqueous solution;
(2) sequentially adding mixed powder and a dispersing agent into the premixed water solution to obtain suspension slurry; the mixed powder comprises ultra-fine diamond and a ceramic bonding agent;
(3) adjusting the pH value of the suspension slurry to 9-11, and then carrying out ball milling to obtain ball milling slurry;
(4) adding a surfactant into the ball-milling slurry, and then stirring and foaming the obtained slurry at a high speed to obtain a wet foam; the high-speed stirring speed is 1000-4000 r/min, and the time is 1-30 min;
(5) adding a catalyst and an initiator into the wet foam, carrying out gel curing on the obtained mixed foam in a mould, covering an organic solvent on the surface of the mixed foam, and demoulding to obtain a porous blank;
(6) and drying and sintering the porous blank in sequence to obtain the ultra-high porosity ceramic bond diamond ultra-precision grinding tool.
According to the invention, an amide organic monomer, a cross-linking agent and water are mixed to obtain a premixed aqueous solution. In the present invention, the amide-based organic monomer is preferably acrylamide or N-vinylpyrrolidone; the cross-linking agent is preferably N, N' -methylene bisacrylamide or polyethylene glycol dimethacrylate; the mass ratio of the amide organic monomer to the cross-linking agent is preferably 1-6: 1, more preferably 4 to 5: 1. The present invention does not require any particular source of the amide-based organic monomer and the crosslinking agent, and commercially available products known to those skilled in the art may be used. In the invention, the mass concentration of the amide organic monomer in the premixed aqueous solution is preferably 1-20%, and more preferably 8-12%. The method for mixing is not particularly required in the invention, and the method well known to those skilled in the art is adopted to ensure that the amide organic monomer, the cross-linking agent and the water are uniformly mixed.
After a premixed aqueous solution is obtained, sequentially adding mixed powder and a dispersing agent into the premixed aqueous solution to obtain suspension slurry; the mixed powder comprises ultra-fine diamond and a ceramic bonding agent. In the present invention, the particle size of the ultra-fine diamond in the mixed powder is preferably 20 μm or less; the granularity of the ceramic bonding agent in the mixed powder is preferably 0.5-10 mu m; the mass ratio of the ultrafine diamond to the ceramic bond is preferably 10-50: 90-50, specifically 1:9, 2:8, 3:7, 4:6 or 5: 5. The present invention does not require any particular kind of ceramic binder, and a diamond ceramic binder well known to those skilled in the art may be used. In the present invention, the mass of the mixed powder is preferably 20 to 60%, more preferably 25 to 45% of the mass of the premixed aqueous solution. In the invention, the dispersing agent preferably comprises one or more of polyacrylic acid, ammonium polymethacrylate, ammonium citrate, tetramethylammonium hydroxide, sodium polyphosphate and ammonium polyacrylate; the mass of the dispersing agent is preferably 1-18% of that of the solid phase, and more preferably 8-17%; after the addition of the dispersant, a stably dispersed suspension slurry was obtained.
After suspension slurry is obtained, the pH value of the suspension slurry is adjusted to 9-11, and then ball milling is carried out to obtain ball milling slurry. The pH value of the suspension slurry is preferably adjusted by adopting ammonia water; the mass concentration of the ammonia water is preferably 25%; the pH value is preferably 9.5-10.5. In the invention, the pH value of the slurry has an important influence on the stability of the slurry, and when the pH value is controlled to be 9-11, the stability of the slurry is good, the slurry is not easy to settle, and the uniform tissue of a subsequently prepared blank body can be ensured. The invention has no special requirements on the ball milling parameters, and can uniformly mix all the components in the suspension slurry.
After ball milling slurry is obtained, the invention adds surfactant into the ball milling slurry, and then the obtained slurry is stirred at high speed and foamed to obtain wet foam. Before adding the surfactant, the invention preferably carries out degassing treatment on the ball milling slurry; the degassing treatment method comprises the following steps: the ball-milled slurry was filtered and then stirred under vacuum. In the invention, the mesh number of the filter screen for filtering is preferably 120-400 meshes; the vacuum degree of the vacuum condition is preferably-0.08 Pa; the rotation speed of stirring under the vacuum condition is preferably 80r/min, and the time of stirring under the vacuum condition is preferably 30 min. The invention removes the bubbles in the ball-milling slurry through degassing treatment, so that the sizes of the bubbles are uniform and controllable in the subsequent high-speed stirring foaming process.
In the present invention, the surfactant preferably includes one or more of Triton X-114, Tween80, sodium Linear Alkylbenzene Sulfonate (LAS), sodium fatty alcohol polyoxyethylene ether sulfate (AES), ammonium fatty alcohol polyoxyethylene ether sulfate (AESA), sodium lauryl sulfate (K12 or SDS), lauroyl glutamic acid, nonylphenol polyoxyethylene ether (TX-10), peregal O, diethanolamide (6501), glycerol monostearate, lignosulfonate, dialkylbenzene sulfonate, alkylsulfonate (petroleum sulfonate), NNO as a dispersing agent, MF as a dispersing agent, PO-EO copolymer and fatty alcohol polyoxyethylene ether (AEO-3); the addition amount of the surfactant in each liter of ball milling slurry is preferably 4-18 g, and more preferably 8-16 g. The source of the surfactant is not particularly required in the present invention, and commercially available products well known to those skilled in the art may be used. In the present invention, the surfactant functions to reduce surface tension, increase the amount of foam generated, and prolong the life of the resulting foam, thereby increasing porosity.
In the invention, the high-speed stirring speed is 1000-4000 r/min, preferably 1000-1500 r/min, and more preferably 1100-1200 r/min; the high-speed stirring time is 1-30 min, preferably 10-18 min, and more preferably 12-15 min. The high-speed stirring mode is not particularly required in the invention, and a mechanical stirring mode well known to those skilled in the art can be adopted. The invention introduces air into the slurry to form a large amount of bubbles by high-speed stirring, thereby obtaining the wet foam.
After the wet foam is obtained, adding a catalyst and an initiator into the wet foam, carrying out gel curing on the obtained mixed foam in a mould, covering the surface of the mixed foam with an organic solvent, and demoulding to obtain a porous blank. In the present invention, the catalyst is preferably N, N' -tetramethylethylenediamine; the initiator is preferably ammonium persulfate; the addition amount of the catalyst is preferably less than or equal to 7.5mL per liter of ball milling slurry; the mass of the initiator is preferably 0.2-3% of the mass of the ball-milling slurry. In the invention, the catalyst and the initiator are preferably uniformly mixed in the wet foam by stirring to obtain mixed slurry. The present invention does not require the mold to be particularly limited, and the mold known to those skilled in the art may be used. In the invention, the time for curing the gel is preferably 3-10 min.
In the present invention, the surface of the mixed foam is covered with a layer of organic solvent, i.e., the density of the organic solvent is lower than that of the mixed foam slurry, and the organic solvent is preferably ethylene glycol or glycerol. According to the invention, the organic solvent is covered on the surface of the mixed foam material, so that the evaporation rate of water in the mixed slurry in the gel curing process can be slowed down, and the defects of cracking and the like of a blank body are avoided. During the process of gel curing, the water in the slurry is slowly volatilized, most of the water is removed, solid-phase substances and organic monomers in the slurry gradually form a three-dimensional network and are solidified into bubble walls, and a large amount of bubbles with uniform sizes are contained in the blank. After the gel is cured, the organic solvent is poured out and demoulded to obtain the porous green body.
After the porous blank is obtained, the porous blank is sequentially dried and sintered to obtain the ultra-high porosity ceramic bond diamond ultra-precision grinding tool. In the present invention, the drying preferably includes room-temperature drying and heat drying which are sequentially performed; the room-temperature drying time is preferably 6-12 hours, and more preferably 8 hours; the heating and drying temperature is preferably 60-100 ℃, and more preferably 80 ℃; the time for heating and drying is preferably 12-24 hours, more preferably 24 hours, and the heating and drying is preferably carried out in a drying oven. According to the invention, the drying rate of the porous blank is controlled by adopting a staged drying mode, so that the porous blank can be ensured not to have drying defects such as cracking and the like. In the invention, the sintering temperature is preferably 450-650 ℃, more preferably 575-625 ℃, and further preferably 600-610 ℃; the sintering heat preservation time is preferably 0.5-1 h, and more preferably 0.6-0.8 h; the heating rate of the sintering is preferably 0.5-1.5 ℃/min, and more preferably 1 ℃/min. In an embodiment of the invention, the sintering is preferably performed in a muffle furnace. In the temperature rise process of sintering, organic matters (polyacrylamide, a dispersing agent, a surfactant, a catalyst and an initiator) in the porous blank are firstly oxidized and lost; then, the ceramic bond gradually undergoes sintering densification; and finally, in the heat preservation process at the sintering temperature, the ceramic bonding agent and the diamond fine particles are well sintered, and the block material with higher strength is obtained.
The method provided by the invention can realize uniform distribution of ultra-fine diamonds and pores in the grinding tool, can enable the porosity in the grinding tool to reach more than 75%, and obviously improves the grinding performance of the ceramic bond diamond ultra-precision grinding tool. In the invention, the size of the air holes in the grinding tool can be effectively controlled by controlling the relative contents of the ultra-fine diamond and the ceramic bond and the rotating speed of high-speed stirring.
The invention provides an ultra-high porosity ceramic bond diamond ultra-precision grinding tool prepared by the preparation method in the scheme, wherein the porosity of the grinding tool is more than or equal to 75%, preferably 75-90%, and the size of pores is 100-350 μm.
The ultra-high porosity vitrified bond diamond ultra-precision grinding tool and the preparation method thereof provided by the present invention will be described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Adding the mixture into deionized water according to the mass ratio of 4:1, preparing Acrylamide (AM) and N, N' -Methylene Bisacrylamide (MBAM) into a premixed aqueous solution, wherein the mass concentration of the acrylamide in the premixed aqueous solution is 8%;
(2) adding mixed powder (diamond/ceramic binder mass ratio is 1:9, diamond particle size is 0.1 μm, ceramic binder particle size is 0.5 μm) and ammonium citrate (TAC) and ammonium polyacrylate (NH)4PAA), the mass of the mixed powder, the mass of the ammonium citrate and the mass of the ammonium polyacrylate are respectively 25%, 1.8% and 2% of the mass of the premixed aqueous solution; by NH3Adjusting the pH value to 9 by ammonia water with the content of 25%, uniformly stirring, and performing ball milling;
(3) milling to obtain ball milling slurry, filtering the slurry with a screen (degassing), and then stirring and degassing under vacuum condition (the rotating speed of a stirrer blade is 80r/min, the vacuum degree is-0.08 Pa, and the degassing time is 30 min); adding 2g of surfactant Triton X-114 into 250mL of ball-milling slurry after degassing, and stirring at a high speed of 1000r/min for 10min to fully foam the mixture to obtain wet foam; adding 240 mu L of catalyst N, N, N ', N' -Tetramethylethylenediamine (TEMED) and initiator Ammonium Persulfate (APS) accounting for 1.0 wt.% of the ball-milling slurry in sequence, and further uniformly stirring;
(4) pouring the slurry into a mould, and covering a layer of organic solvent ethylene glycol with lower density on the surface; after the slurry begins to form gel and is gradually cured into a blank, pouring out the organic solvent and demoulding to obtain a porous blank;
(5) naturally drying the porous blank body at room temperature for 8h, and then drying the porous blank body in a drying oven at 80 ℃ for 24 h; and finally, putting the dried grinding tool sample into a muffle furnace for sintering, wherein the sintering temperature is 575 ℃, and the heat preservation time is 1h, so that the ceramic bond diamond ultra-precision grinding tool with uniformly dispersed diamond and porosity of more than 75% is finally obtained, and the size of pores in the grinding tool is about 320 mu m. (Note: pore size is an average value obtained by SEM observation calculation; porosity is measured based on Archimedes' principle.)
Example 2
(1) Adding acrylamide and N, N' -methylene bisacrylamide in a mass ratio of 4.5:1 into deionized water to prepare a premixed aqueous solution, wherein the mass concentration of the acrylamide in the premixed aqueous solution is 10%;
(2) adding mixed powder (diamond/ceramic bond mass ratio of 2:8, diamond particle size of about 0.25 μm, ceramic bond particle size of about 1.0 μm), ammonium citrate (TAC) and ammonium polyacrylate (NH)4PAA), the mass of the mixed powder, the mass of the ammonium citrate and the mass of the ammonium polyacrylate are respectively 30%, 2.0% and 3% of the mass of the premixed aqueous solution; by NH3Adjusting the pH value to 9.5 by ammonia water with the content of 25%, uniformly stirring, and carrying out ball milling;
(3) milling to obtain ball-milled slurry, filtering the slurry with a screen (degassing), and then stirring and degassing under vacuum condition (the rotating speed of a stirrer blade is 80r/min, the vacuum degree is-0.08 Pa, and the degassing time is 30 min); adding 2.5g of surfactant TritonX-114 into 250mL of ball-milling slurry after degassing, and stirring at a high speed of 1150r/min for 15min to fully foam to obtain wet foam; adding 270 mu L of catalyst N, N, N ', N' -Tetramethylethylenediamine (TEMED) and initiator Ammonium Persulfate (APS) accounting for 1.5 wt.% of the ball-milling slurry in sequence, and further uniformly stirring;
(4) pouring the slurry into a mould, and covering a layer of organic solvent ethylene glycol with lower density on the surface; after the slurry begins to form gel and is gradually cured into a blank, pouring out the organic solvent and demoulding to obtain a porous blank;
(5) naturally drying the porous blank body at room temperature for 8h, and then drying the porous blank body in a drying oven at 80 ℃ for 24 h; and finally, putting the dried grinding tool sample into a muffle furnace for sintering, wherein the sintering temperature is 600 ℃, and the heat preservation time is 0.75h, and finally obtaining the ceramic bond diamond ultra-precision grinding tool with uniformly dispersed diamond and porosity of more than 78%, wherein the size of pores in the grinding tool is about 275 mu m, and the microstructure of the fracture of the grinding tool sample is shown in figure 1.
Example 3
(1) Adding acrylamide and N, N' -methylene bisacrylamide in a mass ratio of 5:1 into deionized water to prepare a premixed aqueous solution, wherein the mass concentration of the acrylamide in the premixed aqueous solution is 12%;
(2) adding mixed powder (diamond/ceramic binder mass ratio of 3:7, diamond particle size of 2.5 μm, and ceramic binder particle size of 5 μm), ammonium citrate (TAC) and ammonium polyacrylate (NH)4PAA), the mass of the mixed powder, the mass of the ammonium citrate and the mass of the ammonium polyacrylate are respectively 40%, 2.5% and 3% of the mass of the premixed aqueous solution; by NH3Adjusting the pH value to 10 by ammonia water with the content of 25%, uniformly stirring, and performing ball milling;
(3) milling to obtain ball-milled slurry, filtering the slurry with a screen (degassing), and then stirring and degassing under vacuum condition (the rotating speed of a stirrer blade is 80r/min, the vacuum degree is-0.08 Pa, and the degassing time is 30 min); adding 3.0g of surfactant Triton X-114 into 250mL of ball-milling slurry after degassing, and stirring at a high speed of 1200r/min for 18min to fully foam the mixture to obtain wet foam; sequentially adding 300 mu L of catalyst N, N, N ', N' -Tetramethylethylenediamine (TEMED) and initiator Ammonium Persulfate (APS) accounting for 1.8 wt.% of the ball-milling slurry, and further uniformly stirring;
(4) pouring the slurry into a mould, and covering a layer of organic solvent ethylene glycol with lower density on the surface; after the slurry begins to form gel and is gradually cured into a blank, pouring out the organic solvent and demoulding to obtain a porous blank;
(5) naturally drying the porous blank body at room temperature for 8h, and then drying the porous blank body in a drying oven at 80 ℃ for 24 h; and finally, putting the dried grinding tool sample into a muffle furnace for sintering at the sintering temperature of 610 ℃ for 0.65h, and finally obtaining the ceramic bond diamond ultra-precision grinding tool with uniformly dispersed diamond and porosity of more than 83%, wherein the size of pores in the grinding tool is about 200 mu m.
Example 4
(1) Adding acrylamide and N, N' -methylene bisacrylamide in a mass ratio of 4:1 into deionized water to prepare a premixed aqueous solution, wherein the mass concentration of the acrylamide in the premixed aqueous solution is 15%;
(2) adding mixed powder (diamond/ceramic binder mass ratio is 4:6, diamond particle size is about 10 μm, and ceramic binder particle size is about 8 μm), ammonium citrate (TAC) and ammonium polyacrylate (NH)4PAA), the mass of the mixed powder, the mass of the ammonium citrate and the mass of the ammonium polyacrylate are respectively 45%, 3.0% and 3.5% of the mass of the premixed aqueous solution; by NH3Adjusting the pH value to 10.5 by ammonia water with the content of 25%, uniformly stirring, and carrying out ball milling;
(3) milling to obtain ball-milled slurry, filtering the slurry with a screen (degassing), and then stirring and degassing under vacuum condition (the rotating speed of a stirrer blade is 80r/min, the vacuum degree is-0.08 Pa, and the degassing time is 30 min); adding 3.6g of surfactant TritonX-114 into 250mL of ball-milling slurry after degassing, and stirring at 1250r/min at a high speed for 20min to fully foam to obtain wet foam; adding 320 mu L of catalyst N, N, N ', N' -Tetramethylethylenediamine (TEMED) and initiator Ammonium Persulfate (APS) accounting for 2.0 wt.% of the ball-milling slurry in sequence, and further uniformly stirring;
(4) pouring the slurry into a mould, and covering a layer of organic solvent ethylene glycol with lower density on the surface; after the slurry begins to form gel and is gradually cured into a blank, pouring out the organic solvent and demoulding to obtain a porous blank;
(5) naturally drying the porous blank body at room temperature for 8h, and then drying the porous blank body in a drying oven at 80 ℃ for 24 h; and finally, putting the dried grinding tool sample into a muffle furnace for sintering at the sintering temperature of 625 ℃ for 0.5h, and finally obtaining the ceramic bond diamond ultra-precision grinding tool with uniformly dispersed diamond and porosity of more than 78%, wherein the size of pores in the grinding tool is about 150 mu m.
Example 5
(1) Adding acrylamide and N, N' -methylene bisacrylamide in a mass ratio of 5:1 into deionized water to prepare a premixed aqueous solution, wherein the mass concentration of the acrylamide in the premixed aqueous solution is 20%;
(2) adding mixed powder (diamond/ceramic binder mass ratio is 5:5, diamond particle size is about 20 μm, and ceramic binder particle size is about 10 μm) and ammonium citrate (TAC) and ammonium polyacrylate (NH)4PAA), the mass of the mixed powder, the mass of the ammonium citrate and the mass of the ammonium polyacrylate are respectively 50 percent, 3.6 percent and 4.0 percent of the mass of the premixed aqueous solution; by NH3Adjusting the pH value to 11 by ammonia water with the content of 25%, uniformly stirring, and performing ball milling;
(3) milling to obtain ball-milled slurry, filtering the slurry with a screen (degassing), and then stirring and degassing under vacuum condition (the rotating speed of a stirrer blade is 80r/min, the vacuum degree is-0.08 Pa, and the degassing time is 30 min); adding 4.0g of surfactant Triton X-114 into 250mL of ball-milling slurry after degassing, and stirring at a high speed of 1500r/min for 30min to fully foam the mixture to obtain wet foam; sequentially adding 350 mu L of catalyst N, N, N ', N' -Tetramethylethylenediamine (TEMED) and initiator Ammonium Persulfate (APS) accounting for 2.5 wt.% of the ball-milling slurry, and further uniformly stirring;
(4) pouring the slurry into a mould, and covering a layer of organic solvent ethylene glycol with lower density on the surface; after the slurry begins to form gel and is gradually cured into a blank, pouring out the organic solvent and demoulding to obtain a porous blank;
(5) naturally drying the porous blank body at room temperature for 8h, and then drying the porous blank body in a drying oven at 80 ℃ for 24 h; and finally, putting the dried grinding tool sample into a muffle furnace for sintering, wherein the sintering temperature is 650 ℃, and the heat preservation time is 0.5h, and finally obtaining the ceramic bond diamond ultra-precision grinding tool with uniformly dispersed diamond and porosity of more than 75%, wherein the size of pores in the grinding tool is about 120 mu m, and the typical micro-morphology of fracture of the grinding tool is similar to that in the graph 1.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A preparation method of an ultra-fine grinding tool of ultra-high porosity ceramic bond diamond comprises the following steps:
(1) mixing an amide organic monomer, a cross-linking agent and water to obtain a premixed aqueous solution;
(2) sequentially adding mixed powder and a dispersing agent into the premixed water solution to obtain suspension slurry; the mixed powder comprises ultra-fine diamond and a ceramic bonding agent;
(3) adjusting the pH value of the suspension slurry to 9-11, and then carrying out ball milling to obtain ball milling slurry; adjusting the pH value of the slurry of the suspension by using ammonia water;
(4) adding a surfactant into the ball-milling slurry, and then stirring and foaming the obtained slurry at a high speed to obtain a wet foam; the high-speed stirring speed is 1000-4000 r/min, and the time is 1-30 min;
(5) adding a catalyst and an initiator into the wet foam, carrying out gel curing on the obtained mixed foam in a mould, covering an organic solvent on the surface of the mixed foam, and demoulding to obtain a porous blank;
(6) and drying and sintering the porous blank in sequence to obtain the ultra-high porosity ceramic bond diamond ultra-precision grinding tool.
2. The preparation method according to claim 1, wherein the amide-based organic monomer in step (1) is acrylamide or N-vinylpyrrolidone;
the cross-linking agent is N, N' -methylene bisacrylamide or polyethylene glycol dimethacrylate;
the mass ratio of the amide organic monomer to the cross-linking agent is 1-6: 1.
3. the preparation method according to claim 1 or 2, wherein the mass concentration of the amide-based organic monomer in the premixed aqueous solution of step (1) is 1-20%.
4. The method according to claim 1, wherein the mixed powder of step (2) has a particle size of the ultra-fine diamond of 20 μm or less and a particle size of the ceramic binder of 0.5 to 10 μm; the mass ratio of the superfine diamond to the ceramic bond is 10-50: 90-50; the mass of the mixed powder is 20-60% of that of the premixed water solution.
5. The method according to claim 1 or 4, wherein the dispersant of step (2) comprises one or more of polyacrylic acid, ammonium polymethacrylate, ammonium citrate, tetramethylammonium hydroxide, sodium polyphosphate and ammonium polyacrylate; the mass of the dispersing agent is 1-18% of the mass of the mixed powder.
6. The preparation method according to claim 1, wherein the step (4) further comprises degassing the ball-milling slurry before adding the surfactant; the degassing treatment method comprises the following steps: the ball-milled slurry was filtered and then stirred under vacuum.
7. The preparation method according to claim 1 or 6, wherein the surfactant in step (4) comprises one or more of Triton X-114, Tween80, sodium linear alkylbenzene sulfonate, sodium fatty alcohol-polyoxyethylene ether sulfate, ammonium fatty alcohol-polyoxyethylene ether sulfate, sodium lauryl sulfate, lauroyl glutamic acid, polyoxyethylene nonylphenol ether, peregal O, diethanolamide, glyceryl monostearate, lignosulfonate, heavy alkylbenzene sulfonate, alkylsulfonate, NNO as a dispersing agent, MF as a dispersing agent, PO-EO copolymer and fatty alcohol-polyoxyethylene ether; the addition amount of the surfactant in each liter of ball milling slurry is 4-18 g.
8. The production method according to claim 1, wherein the catalyst in the step (5) is N, N, N ', N' -tetramethylethylenediamine; the initiator is ammonium persulfate; the catalyst is added in an amount of less than or equal to 7.5mL per liter of ball-milling slurry; the mass of the initiator is 0.2-3% of that of the ball-milling slurry.
9. The production method according to claim 1, wherein the drying in the step (6) includes room-temperature drying and heat drying which are sequentially performed; the drying time at room temperature is 6-12 h; the heating and drying temperature is 60-100 ℃, and the time is 12-24 hours;
the sintering temperature is 450-650 ℃, and the heat preservation time is 0.5-1 h.
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| CN113997213B (en) * | 2020-10-16 | 2023-06-20 | 安泰科技股份有限公司 | Ceramic diamond grinding wheel for thinning SiC wafer and manufacturing method thereof |
| CN113199412B (en) * | 2021-04-24 | 2022-03-08 | 无锡希必恩精密工具有限公司 | Superhard CBN (cubic boron nitride) ceramic grinding wheel and preparation method thereof |
| CN114750081B (en) * | 2022-04-06 | 2024-04-02 | 郑州跃川超硬材料有限公司 | Ceramic bond with air holes and preparation method thereof |
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