CN112692956A - Slurry direct-writing forming method of honeycomb-shaped diamond tool - Google Patents

Slurry direct-writing forming method of honeycomb-shaped diamond tool Download PDF

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CN112692956A
CN112692956A CN202011586855.9A CN202011586855A CN112692956A CN 112692956 A CN112692956 A CN 112692956A CN 202011586855 A CN202011586855 A CN 202011586855A CN 112692956 A CN112692956 A CN 112692956A
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honeycomb
slurry
sintering
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diamond tool
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CN112692956B (en
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陆静
王艳辉
黄景銮
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Huaqiao University
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Abstract

The invention discloses a slurry direct-writing forming method of a honeycomb-shaped diamond tool, wherein the honeycomb-shaped diamond tool is a cylinder with the diameter of 80-150mm and the height of 50-120mm, the upper top surface and the lower top surface of the honeycomb-shaped diamond tool are provided with a plurality of hexagonal honeycomb-shaped through holes, the side length of each hexagonal honeycomb-shaped through hole is 2-3mm, and the total area occupied by the hexagonal honeycomb-shaped through holes is 30-40% of the total area of the upper top surface of the cylinder. The invention can prepare the complex honeycomb structure which is difficult to form by the traditional method, and can adjust the printing size of the honeycomb holes according to the grinding requirement, the porous honeycomb structures can improve the space for containing and discharging chips, effectively remove the chips generated by grinding, accelerate the heat dissipation, have good self-sharpening property and avoid the heat damage caused by blockage.

Description

Slurry direct-writing forming method of honeycomb-shaped diamond tool
Technical Field
The invention belongs to the technical field of grinding tool materials, and particularly relates to a slurry direct-writing forming method of a honeycomb-shaped diamond tool.
Background
With the development of ultra-precision grinding technology, higher requirements are put forward on the processing efficiency and the processing quality of the grinding wheel. The ceramic bond diamond grinding wheel with the porous structure has the advantages of good self-sharpening property, large chip removal space, small grinding force and the like in the using process, and has obvious advantages in grinding materials with high hardness, large brittleness and high precision requirement, such as semiconductor substrates, hard alloys, novel ceramics and the like. In the prior art, a diamond tool is mainly prepared in a hot-press forming mode, the traditional hot-press forming method utilizes dry mixing to easily agglomerate, and the requirement of high-quality grinding tracks cannot be met by manually pressing simple shapes. In addition, the pore-forming agent is added in the hot press forming, the pore-forming agent is completely decomposed to generate pores during sintering, the prepared pores belong to passive forming, and the size and the shape of the pores are difficult to control due to factors such as the accumulation of the pore-forming agent, deformation in the combustion process and the like. Any complex structure can be prepared by using the additive manufacturing technology, and the automation degree is improved.
The currently common 3D printing technology comprises SLM and SLS, the SLM and SLS technology can print a diamond tool with a cooling inner flow channel, but the two methods both need to adopt laser high-temperature sintering to be more than 1000 ℃, diamond micro powder is graphitized when being sintered to be more than 700 ℃, and the laser layer-by-layer sintering has the defects of uneven sintering quality and the like. The wet method mixed powder does not have agglomeration by using a slurry direct writing forming technology, and the honeycomb diamond tool can be printed and then sintered to integrally form an integral structure. However, the conventional ceramic bond powder in the slurry direct-writing forming technology is SiO2As a main component, the shape and size change after sintering is large, and a good honeycomb structure cannot be maintained. And the ceramic bond powder particles are micron-sized, and the powder particles are even larger than the diamond grinding material, so that the diamond micro powder cannot be completely wrapped, and the bonding strength is low.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a slurry direct-writing forming method of a honeycomb-shaped diamond tool.
The technical scheme of the invention is as follows:
a slurry direct writing forming method of a honeycomb-shaped diamond tool is characterized in that the honeycomb-shaped diamond tool is a cylinder with the diameter of 80-150mm and the height of 50-120mm, the upper top surface and the lower top surface of the cylinder are provided with a plurality of hexagonal honeycomb-shaped through holes, the side length of each hexagonal honeycomb-shaped through hole is 2-3mm, and the total area occupied by the hexagonal honeycomb-shaped through holes is 30-40% of the total area of the upper top surface of the cylinder;
the method specifically comprises the following steps:
(1) fully mixing nano ceramic powder with a melting point of 655-665 ℃ and diamond microparticles in a ratio of 70-80 wt% to 20-30 wt% to obtain mixed powder; the nano ceramic powder comprises the following raw materials: 64-65 parts of silicon powder, 5.8-6.3 parts of sodium oxide, 9-12 parts of aluminum oxide, 2.9-3.3 parts of potassium oxide and 10-11 parts of boron trioxide; (2) fully dispersing chitosan in deionized water to obtain a chitosan solution with the concentration of 2.8-3.1 wt%;
(3) uniformly mixing the mixed powder prepared in the step (1) with the chitosan solution obtained in the step (2) to obtain slurry, wherein the volume ratio of the mixed powder to the chitosan solution is 69-70% to 30-31%;
(4) adding the slurry prepared in the step (3) into a needle cylinder of slurry direct-writing forming equipment, and printing the slurry into a designed shape in a layer-by-layer overlapping mode to obtain a blank body;
(5) and (5) drying the green body prepared in the step (4) to constant weight, and sintering to obtain the honeycomb-shaped diamond tool.
In a preferred embodiment of the present invention, the diamond microparticles have a particle size of 5 to 40 μm.
In a preferred embodiment of the present invention, the raw material of the nano ceramic powder consists of 65 parts by weight of silicon powder, 6 parts by weight of sodium oxide, 12 parts by weight of aluminum oxide, 3 parts by weight of potassium oxide and 11 parts by weight of diboron trioxide, and has a melting point of 660 ℃.
In a preferred embodiment of the invention, the concentration of the chitosan solution is 3 wt%.
In a preferred embodiment of the invention, the volume ratio of the mixed powder to the chitosan solution is 69% to 31%.
In a preferred embodiment of the present invention, the printing process parameters are: the printing speed of the needle head is 3-10mm/s, the radius of the nozzle is 1.4-1.6mm, the shearing rate is 10-30/s, the flow rate is 80-120%, and the temperature is 20-35 ℃.
Further preferably, the printing process parameters are as follows: the printing speed of the needle head is 4mm/s, the radius of the nozzle is 1.5mm, the shearing rate is 10.6/s, the flow rate is 120 percent, and the temperature is 25 ℃.
In a preferred embodiment of the present invention, the sintering is specifically: sending the blank dried to constant weight into a sintering atmosphere furnace, heating from room temperature to 300-320 ℃ at the heating rate of 2-3 ℃/min in the air atmosphere, and preserving heat for 50-60 min; then heating to 655-665 ℃ at the heating rate of 3-5 ℃/min under the argon atmosphere, and carrying out heat preservation sintering for 60-90 min; then cooling to room temperature along with the furnace.
Further preferably, the sintering specifically comprises: sending the blank dried to constant weight into a sintering atmosphere furnace, sending into the sintering atmosphere furnace, heating from room temperature to 300 ℃ at a heating rate of 2.5 ℃/min in the air atmosphere, and keeping the temperature for 60 min; then heating to 660 ℃ at the heating rate of 4 ℃/min under the argon atmosphere, and carrying out heat preservation sintering for 90 min; then cooling to room temperature along with the furnace.
In a preferred embodiment of the invention, the drying is in air for 20-40 h.
The invention has the beneficial effects that:
1. the invention can prepare the complex honeycomb structure which is difficult to form by the traditional method, and can adjust the printing size of the honeycomb holes according to the grinding requirement, the porous honeycomb structures can improve the space for containing and discharging chips, effectively remove the chips generated by grinding, accelerate the heat dissipation, have good self-sharpening property and avoid the heat damage caused by blockage.
2. According to the invention, potassium oxide and boron trioxide are added into the nano ceramic powder in a certain proportion, so that the melting point of the nano ceramic powder reaches 655-665 ℃; the nano ceramic powder in the invention takes silicon powder as a main component, part of the silicon powder is oxidized into silicon dioxide in the sintering process to expand in volume so as to offset the volume shrinkage caused by other components, and the size change rate of the sintered diamond tool is less than 0.5 percent.
3. According to the invention, the chitosan solution with specific concentration and specific volume is added, so that the viscosity and the storage modulus of the powder slurry can be improved, the requirement of extrusion molding is met, and the formed body is prevented from collapsing.
4. The invention has high material utilization rate.
Drawings
FIG. 1 is a graph of viscosity as a function of shear rate for slurries of different chitosan content in example 3 of the present invention.
Fig. 2 is a schematic view showing the structure of the honeycomb diamond tool prepared in examples 3 and 4 of the present invention.
FIG. 3 is a photograph showing slurries containing different proportions of chitosan solutions according to example 3 of the present invention after direct-write molding of the slurries, wherein (a) the 28% chitosan solution, (b) the 30% chitosan solution, and (c) the 35% chitosan solution.
Detailed Description
The technical solution of the present invention will be further illustrated and described below with reference to the accompanying drawings by means of specific embodiments.
Example 1
(1) Mixing silicon powder, sodium oxide, aluminum oxide, potassium oxide and boron trioxide in the following weight parts shown in the table 1 for 4 hours at a rotating speed of 600r/min by using a mixer to obtain nano ceramic powder;
TABLE 1
Figure BDA0002865059120000031
Figure BDA0002865059120000041
(2) Fully dispersing chitosan in deionized water (stirring for 90min at the rotating speed of 800r/min by using a stirrer) to obtain a chitosan solution with the concentration of 3 wt%;
(3) uniformly mixing the nano ceramic powder prepared in the step (1) with the chitosan solution obtained in the step (2) to obtain slurry, wherein the volume ratio of the mixed powder to the chitosan solution is 69: 31%;
(4) adding the slurry prepared in the step (3) into a needle cylinder of slurry direct-writing forming equipment, and printing the slurry into a designed shape in a layer-by-layer overlapping mode to obtain a blank body; the printing process parameters are as follows: the printing speed of a needle head is 4mm/min, the radius of a nozzle is 1.5mm, the shearing rate is 10.6/s, the flow rate is 120 percent, and the temperature is 25 ℃;
(5) drying the blank prepared in the step (4) for 48h in an air atmosphere to constant weight, then sending the blank into a sintering atmosphere furnace, and raising the temperature from room temperature to 300 ℃ at a temperature raising speed of 2.5 ℃/min in the air atmosphere as shown in figure 1, and preserving the temperature for 60 min; then heating to 660 ℃ at the heating rate of 4 ℃/min under the argon atmosphere, and carrying out heat preservation sintering for 90 min; and then cooling to room temperature along with the furnace to obtain the diamond tool (without honeycomb through holes), wherein the diamond tool is a cylinder with the diameter of 120mm and the height of 60 mm. The properties of the diamond tools made from the nano-ceramic powders of different formulations in table 1 are shown in table 2 below:
TABLE 2
Numbering Dimensional Change Rate (%) Bending strength (MPa) Compressive strength (MPa) Melting Point (. degree.C.)
1 0.19 58.6 51.3 700
2 0.17 59.5 53.4 710
3 0.16 60.2 54.5 725
4 0.13 63.7 58.2 750
5 0.18 54.4 48.3 660
6 0.16 56.3 51.2 680
7 0.14 59.8 54.5 690
Example 2
(1) Mixing silicon powder, sodium oxide, aluminum oxide, potassium oxide and boron trioxide in the following weight parts shown in the following table 3 for 4 hours at a rotating speed of 600r/min by using a mixer to obtain nano ceramic powder;
TABLE 3
Serial number Silicon powder Sodium oxide Alumina oxide Potassium oxide Boron trioxide
1 65 6 12 3 11
2 63 6 12 3 11
3 61 6 12 3 11
4 59 6 12 3 11
The properties of the diamond tools manufactured by using the nano ceramic powders of different formulations in the same manner as in example 1 and table 3 in the steps (2) to (5) are shown in table 4 below:
TABLE 4
Numbering Dimensional Change Rate (%) Bending strength (MPa) Compressive strength (MPa)
1 0.17 56.3 51.2
2 0.29 55.1 49.6
3 0.38 53.7 48.9
4 0.46 50.6 46.2
By combining the data of the example 1, the melting point of the selected nano ceramic powder is determined to be 660 ℃, and the specific formula of the nano ceramic powder is as follows: 65 parts by weight of silicon powder, 6 parts by weight of sodium oxide, 12 parts by weight of aluminum oxide, 3 parts by weight of potassium oxide, and 11 parts by weight of diboron trioxide.
Example 3
(1) Mixing the nano ceramic powder determined in example 2 and W10 diamond microparticles (10 μm) in a ratio of 75 wt% to 25 wt% at a rotation speed of 600r/min for 4h to obtain a mixed powder;
(2) fully dispersing chitosan in deionized water (stirring for 90min at the rotating speed of 800r/min by using a stirrer) to obtain a chitosan solution with the concentration of 3 wt%;
(3) uniformly mixing the mixed powder prepared in the step (1) with the chitosan solution obtained in the step (2) to obtain slurry, wherein the volume percentages of the chitosan solution and the mixed powder are respectively 28: 72%, 31: 69% and 35: 65%;
(4) adding the slurry prepared in the step (3) into a needle cylinder of slurry direct-writing forming equipment, and printing the slurry into a designed shape in a layer-by-layer (layer thickness is 1mm) overlapping mode to obtain a blank body; the printing process parameters are as follows: the printing speed of a needle head is 4mm/s, the radius of a nozzle is 1.5mm, the shearing rate is 10.6/s, the flow rate is 120 percent, and the temperature is 25 ℃;
(5) drying the blank prepared in the step (4) for 48h in an air atmosphere to constant weight, then sending the blank into a sintering atmosphere furnace, heating the blank from room temperature to 300 ℃ at a heating rate of 2.5 ℃/min in an argon atmosphere, preserving heat for 60min, heating the blank to 660 ℃ at a heating rate of 4 ℃/min, preserving heat and sintering for 90 min; and then cooling to room temperature along with the furnace to obtain the honeycomb-shaped diamond tool, wherein the honeycomb-shaped diamond tool is a cylinder with the diameter of 120mm and the height of 60mm, the upper top surface and the lower top surface of the cylinder are provided with a plurality of hexagonal honeycomb-shaped through holes, and the side length of the hexagonal honeycomb-shaped through holes is 2mm, as shown in figure 2. As shown in fig. 1, the viscosity of the corresponding slurry was 46524mPa · s, 41862mPa · s, 25763mPa · s in this order, and the viscosity of the slurry decreased with increasing shear rate, showing shear thinning behavior. As shown in fig. 3, the diamond tool manufactured according to the slurry of 31% by volume of chitosan solution in this example was stably formed and the shape was well maintained. The viscosity of the slurry with 28% of chitosan solution by volume is larger, and partial cracks exist after printing; the 35% by volume of chitosan solution had a relatively low viscosity and could not be molded as a whole after printing.
Example 4
(1) Mixing the nano ceramic powder determined in example 2 and W10 diamond microparticles (10 μm) in a ratio of 75 wt% to 25 wt% at a rotation speed of 600r/min for 4h to obtain a mixed powder;
(2) fully dispersing chitosan in deionized water (stirring for 90min at the rotating speed of 800r/min by using a stirrer) to obtain a chitosan solution with the concentration of 3 wt%;
(3) uniformly mixing the mixed powder prepared in the step (1) with the chitosan solution obtained in the step (2) to obtain slurry, wherein the volume ratio of the mixed powder to the chitosan solution is 69: 31%;
(4) adding the slurry prepared in the step (3) into a needle cylinder of slurry direct-writing forming equipment, and printing the slurry into a designed shape in a layer-by-layer (layer thickness is 1mm) overlapping mode to obtain a blank body; the printing process parameters are as follows: the printing speed of a needle head is 4mm/s, the radius of a nozzle is 1.5mm, the shearing rate is 10.6/s, the flow rate is 120 percent, and the temperature is 25 ℃;
(5) drying the blank prepared in the step (4) for 48h in an air atmosphere to constant weight, then sending the blank into a sintering atmosphere furnace, heating the blank from room temperature to 300 ℃ at a heating rate of 2.5 ℃/min in an argon atmosphere, preserving heat for 60min, heating the blank to 660 ℃ at a heating rate of 4 ℃/min, preserving heat and sintering for 90 min; and then cooling to room temperature along with the furnace to obtain the honeycomb-shaped diamond tool, wherein the honeycomb-shaped diamond tool is a cylinder with the diameter of 120mm and the height of 60mm, the upper top surface and the lower top surface of the cylinder are provided with a plurality of hexagonal honeycomb-shaped through holes, and the side length of the hexagonal honeycomb-shaped through holes is 2mm, as shown in figure 2. The diamond tools without the hexagonal honeycomb through holes are prepared by repeating the steps (1) to (5), the performances of the two diamond tools are compared, as shown in the following table 5, and the honeycomb diamond tool prepared by the embodiment saves 31% of raw materials compared with the diamond tool without the hexagonal honeycomb through holes.
TABLE 5
Figure BDA0002865059120000061
Figure BDA0002865059120000071
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.

Claims (10)

1. A slurry direct-writing forming method of a honeycomb-shaped diamond tool is characterized by comprising the following steps:
the honeycomb diamond tool is a cylinder with the diameter of 80-150mm and the height of 50-120mm, the upper top surface and the lower top surface of the cylinder are provided with a plurality of hexagonal honeycomb through holes, the side length of each hexagonal honeycomb through hole is 2-3mm, and the total area occupied by the hexagonal honeycomb through holes is 30-40% of the total area of the upper top surface of the cylinder;
the method specifically comprises the following steps:
(1) fully mixing nano ceramic powder with a melting point of 655-665 ℃ and diamond microparticles in a ratio of 70-80 wt% to 20-30 wt% to obtain mixed powder; the raw materials of the nano ceramic powder consist of 64 to 65 weight portions of silicon powder, 5.8 to 6.3 weight portions of sodium oxide, 9 to 12 weight portions of aluminum oxide, 2.9 to 3.3 weight portions of potassium oxide and 10 to 11 weight portions of boron trioxide;
(2) fully dispersing chitosan in deionized water to obtain a chitosan solution with the concentration of 2.8-3.1 wt%;
(3) uniformly mixing the mixed powder prepared in the step (1) with the chitosan solution obtained in the step (2) to obtain slurry, wherein the volume ratio of the mixed powder to the chitosan solution is 69-70% to 30-31%;
(4) adding the slurry prepared in the step (3) into a needle cylinder of slurry direct-writing forming equipment, and printing the slurry into a designed shape in a layer-by-layer overlapping mode to obtain a blank body;
(5) and (5) drying the green body prepared in the step (4) to constant weight, and sintering to obtain the honeycomb-shaped diamond tool.
2. The slurry direct write molding method according to claim 1, characterized in that: the particle size of the diamond microparticles is 5-40 μm.
3. The slurry direct write molding method according to claim 1, characterized in that: the raw materials of the nano ceramic powder consist of 65 weight parts of silicon powder, 6 weight parts of sodium oxide, 12 weight parts of aluminum oxide, 3 weight parts of potassium oxide and 11 weight parts of diboron trioxide, and the melting point of the nano ceramic powder is 660 ℃.
4. The slurry direct write molding method according to claim 1, characterized in that: the concentration of the chitosan solution was 3 wt%.
5. The slurry direct write molding method according to claim 1, characterized in that: the volume ratio of the mixed powder to the chitosan solution is 69 percent to 31 percent.
6. The direct-write slurry forming method according to any one of claims 1 to 5, wherein: the printing process parameters are as follows: the printing speed of the needle head is 3-10mm/s, the radius of the nozzle is 1.4-1.6mm, the shearing rate is 10-30/s, the flow rate is 80-120%, and the temperature is 20-35 ℃.
7. The slurry direct write molding method according to claim 6, characterized in that: the printing process parameters are as follows: the printing speed of the needle head is 4mm/s, the radius of the nozzle is 1.5mm, the shearing rate is 10.6/s, the flow rate is 120 percent, and the temperature is 25 ℃.
8. The direct-write slurry forming method according to any one of claims 1 to 5, wherein: the sintering specifically comprises the following steps: sending the blank dried to constant weight into a sintering atmosphere furnace, heating from room temperature to 320 ℃ at the heating rate of 2-3 ℃/min under the argon atmosphere, preserving heat for 50-60min, then heating to 655 ℃ at the heating rate of 3-5 ℃/min, preserving heat for sintering for 60-90min, and then cooling to room temperature along with the furnace.
9. The slurry direct write molding method according to claim 8, characterized in that: the sintering specifically comprises the following steps: sending the blank dried to constant weight into a sintering atmosphere furnace, sending into the sintering atmosphere furnace, heating from room temperature to 300 ℃ at the heating rate of 2.5 ℃/min under the argon atmosphere, preserving heat for 60min, then heating to 660 ℃ at the heating rate of 4 ℃/min, preserving heat and sintering for 90 min; then cooling to room temperature along with the furnace.
10. The direct-write slurry forming method according to any one of claims 1 to 5, wherein: the drying is carried out in the air for 20-40 h.
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CN114274060A (en) * 2021-11-23 2022-04-05 北京安泰钢研超硬材料制品有限责任公司 Metal-based diamond tool bit for thinning high-end SiC chip, grinding wheel and manufacturing method of metal-based diamond tool bit
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CN116947524A (en) * 2023-09-20 2023-10-27 华侨大学 Laser curing forming method of ceramic bond fine-grained diamond honeycomb grinding block

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CN116947524B (en) * 2023-09-20 2023-12-22 华侨大学 Laser curing forming method of ceramic bond fine-grained diamond honeycomb grinding block

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