CN113716560A - Method for etching surface of artificial diamond - Google Patents
Method for etching surface of artificial diamond Download PDFInfo
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- CN113716560A CN113716560A CN202110800050.8A CN202110800050A CN113716560A CN 113716560 A CN113716560 A CN 113716560A CN 202110800050 A CN202110800050 A CN 202110800050A CN 113716560 A CN113716560 A CN 113716560A
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Abstract
The invention provides a method for etching the surface of a synthetic diamond, which is carried out under the condition that the vacuum degree is 5.0 multiplied by 10‑3Pa～5.0×10‑4Under the Pa condition, according to a set condition, heating a mixture of metal titanium powder and diamond particles to 850-1000 ℃, preserving heat for 30-120 min, then carrying out acid cleaning, cleaning and drying to realize etching on the surface of the diamond, wherein graphitization does not occur in the etching process, and the maximum specific surface area of the etched diamond can reach 0.31m2·g‑1The diamond and binder etched using the method had a 56% increase in maximum bending strength over the untreated diamond.
Description
Technical Field
The invention relates to the technical field of diamond surface treatment, in particular to a method for etching the surface of an artificial diamond.
Background
The diamond grinding tool is a product which is made of diamond as a grinding material by means of a bonding agent and other auxiliary materials and has certain shape, performance and application. However, the surface energy of the artificially synthesized diamond particles is high and is not easy to be wetted by the bonding agent material, so that the diamond and the bonding agent are basically not chemically bonded, and the mechanical inlaying of the bonding agent to the diamond is mainly used. And because the surface of the diamond is smooth, the mechanical bonding force between the bonding agent and the diamond is weak, in the actual grinding process, the diamond particles fall off in advance before the grinding effect of the diamond particles is not fully exerted, the cutting efficiency of the diamond tool is reduced, the service life of the diamond tool is shortened, and the processing cost is improved.
In order to improve the interface bonding force between the diamond and the bonding agent material, the method adopted at present mainly comprises the steps of plating or coating metal, micro-powder corundum and organic treatment on the surface of the diamond, and etching the surface of the diamond. Wherein, the diamond surface is plated or coated with metal, micro-powder corundum and organized, and the bonding force between the diamond and the substrate is poor due to the characteristics of high surface energy and poor wettability of the diamond; compared with the method, the existing method for etching the diamond surface can improve the bonding strength of the diamond and the substrate.
Currently, etching methods include, for example, metal etching, molten salt etching, plasma etching, etc., wherein metal etching is considered as the best method for etching diamond due to its simple operation and low cost. However, in view of the fact that metals such as iron, nickel, cobalt and the like are often selected as catalysts in the preparation process of the artificial diamond, and in the metal etching process, the diamond is graphitized due to the adoption of the metals, so that the mechanical properties of the diamond are reduced, and a good etching effect cannot be obtained.
Disclosure of Invention
In order to solve the problems, the invention provides a method for etching the surface of the artificial diamond.
The main content of the invention comprises:
a method of etching a surface of a synthetic diamond, comprising the steps of:
s1, uniformly mixing dried diamond particles and metal titanium powder with the particle size of 40-50 mu m in a mass ratio of 1: 1-1: 3, and then putting the mixture into a ceramic crucible;
s2, placing the ceramic crucible into a vacuum furnace, and pumping the vacuum degree to 5.0 multiplied by 10-4Pa～5.0×10-3Pa, heating to 750 ℃ at a heating rate of 10 ℃/min, preserving heat for 10min, then heating to 850-1000 ℃ at a heating rate of 5 ℃/min, preserving heat for 30-120 min, and then cooling to room temperature along with the furnace;
and S3, treating the product obtained in the step S2 by using a hydrofluoric acid solution, then placing the product in aqua regia for heating and soaking, finally washing the product by using deionized water until the washing liquid is neutral, and drying the washing liquid to obtain the diamond particles with etching pits on the surfaces.
Preferably, a pretreatment step of the diamond surface is further included before S1.
Preferably, the diamond surface pretreatment step comprises: ultrasonically cleaning diamond particles with the particle size of 40-45 mu m in acetone for 30min, then ultrasonically cleaning in deionized water, and drying for S1.
Preferably, S2 is heated to 850-100 ℃ in a sectional heating mode.
Preferably, the sectional heating mode comprises a first-stage heating process and a second-stage heating process, wherein the first-stage heating process is as follows: heating to 750 ℃ at the heating rate of T1, and keeping the temperature for T1 time; and the second stage of heating process is to heat to 850-1000 ℃ at the temperature rising rate of T2, and to preserve heat for T2 time, wherein T1 is more than T2, and T1 is more than T2.
Preferably, the hydrofluoric acid solution used in S3 is a mixed solution in which the volume ratio of hydrofluoric acid to water is 1: 2.
The invention has the beneficial effects that: the invention provides a method for etching the surface of an artificial diamond, which realizes the etching of the surface of the diamond under the vacuum condition and the certain temperature condition through metal titanium powder, the graphitization can not occur in the etching process, and the specific surface area of the diamond after etching can reach 0.31m to the maximum2·g-1The maximum bending strength of diamond and adhesive etched using the method was increased by 56% compared to untreated diamond.
Drawings
FIG. 1 is a schematic diagram of an etching process of the present invention;
FIG. 2 is a graph of the original topography of an experimental diamond;
FIG. 3 is a topographical view of the etched diamond of the first embodiment;
FIG. 4 is a topographical view of the etched diamond of example two;
FIG. 5 is a topographical view of the etched diamond of example III;
FIG. 6 is a topographical view of the etched diamond of the fourth example;
FIG. 7 is a topographical view of the etched diamond of example V;
FIG. 8 is an XPS spectrum of a raw diamond;
FIG. 9 is an XPS spectrum of diamond after five etches in example;
FIG. 10 is a graphical representation of the specific surface area of diamond as a function of temperature;
FIG. 11 is a bar graph of the bending strength of the pentaphenolic resin-based binder of the example with virgin diamond and etched diamond at different temperature conditions, respectively.
Detailed Description
The technical scheme protected by the invention is specifically explained in the following by combining the attached drawings.
The method for etching the surface of the diamond comprises a pretreatment step, a uniformly-mixed vacuum heating step, an acid cleaning step and a cleaning and drying step, and with reference to fig. 1, firstly, the original diamond is cleaned by acetone to clean the surface of the diamond, then uniformly mixing the diamond particles and the metal titanium powder according to a set proportion, putting the mixture into a ceramic crucible, putting the ceramic crucible containing the mixture of the diamond particles and the metal titanium powder into a vacuum furnace for heating, the vacuum degree in the vacuum furnace needs to reach a set condition, the vacuum furnace is heated to a set temperature at a certain heating rate in a sectional heating mode, the temperature is kept for a certain time, the vacuum furnace is cooled to room temperature along with the furnace, and then cleaning with hydrofluoric acid solution, heating and soaking in aqua regia, washing with deionized water to neutrality, and drying to obtain the diamond particles with etching pits on the surface.
Examples of the experiments
Example 1
(1) Weighing 5g of diamond particles with the particle size of 40-45 meshes, ultrasonically cleaning the diamond particles in acetone for 30min to remove impurities on the surfaces of the diamond particles, then ultrasonically cleaning the diamond particles in deionized water, and drying the diamond particles for use;
(2) uniformly mixing the cleaned diamond particles and metal titanium powder (the particle size is 40-50 mu m) in a mass ratio of 1:2, putting the mixture into a ceramic crucible, then putting the ceramic crucible into a vacuum furnace, and pumping the vacuum degree to 5 x 10-3Heating was started after Pa. Firstly, heating to 750 ℃ at the heating rate of 10 ℃/min, and preserving heat for 10 min; then heating to 850 ℃ at the heating rate of 5 ℃/min, preserving the heat for 30min, and then cooling to the room temperature along with the furnace;
(3) and (4) carrying out acid washing treatment on the heated product. Firstly, preparing a hydrofluoric acid solution according to the volume ratio of hydrofluoric acid to water =1:2, and removing residual metal titanium by using the prepared hydrofluoric acid solution; then, aqua regia is prepared according to the volume ratio of nitric acid to hydrochloric acid =1:3, and residual reactants on the surfaces of the diamond particles are removed through heating and soaking; and finally, washing the diamond particles by using deionized water until the washing liquid is neutral, and drying to obtain the diamond particles with etching pits on the surfaces, wherein the surface appearance of the obtained diamond is shown in figure 3.
Example 2
(1) Weighing 5g of diamond particles with the particle size of 40-45 meshes, ultrasonically cleaning the diamond particles in acetone for 30min to remove impurities on the surfaces of the diamond particles, then ultrasonically cleaning the diamond particles in deionized water, and drying the diamond particles for use;
(2) uniformly mixing the cleaned diamond particles and metal titanium powder (the particle size is 40-50 mu m) in a mass ratio of 1:2, putting the mixture into a ceramic crucible, then putting the ceramic crucible into a vacuum furnace, and pumping the vacuum degree to 5 x 10-3Heating was started after Pa. Heating to 750 deg.C at a heating rate of 10 deg.C/min, and maintaining for 10 min; then heating to 950 ℃ at the heating rate of 5 ℃/min, preserving the heat for 30min, and then cooling to room temperature along with the furnace;
(3) performing acid cleaning treatment on the heated product, preparing a hydrofluoric acid solution according to the volume ratio of hydrofluoric acid to water =1:2, and removing residual metal titanium by using the prepared hydrofluoric acid solution; then, aqua regia is prepared according to the volume ratio of nitric acid to hydrochloric acid =1:3, and residual reactants on the surfaces of the diamond particles are removed through heating and soaking; and finally, washing the diamond particles by using deionized water until the washing liquid is neutral, and drying to obtain the diamond particles with etching pits on the surfaces, wherein the surface appearance of the obtained diamond is shown in figure 4.
Example 3
(1) Weighing 5g of diamond particles with the particle size of 40-45 meshes, ultrasonically cleaning the diamond particles in acetone for 30min to remove impurities on the surfaces of the diamond particles, then ultrasonically cleaning the diamond particles in deionized water, and drying the diamond particles for use;
(2) uniformly mixing the cleaned diamond particles and metal titanium powder (the particle size is 40-50 mu m) in a mass ratio of 1:3, putting the mixture into a ceramic crucible, then putting the ceramic crucible into a vacuum furnace, and pumping the vacuum degree to 5 x 10-3Heating was started after Pa. Heating to 750 deg.C at a heating rate of 10 deg.C/min, and maintaining for 10 min; then heating to 950 ℃ at the heating rate of 5 ℃/min, preserving the heat for 30min, and then cooling to room temperature along with the furnace;
(3) and (4) carrying out acid washing treatment on the heated product. Firstly, preparing a hydrofluoric acid solution according to the volume ratio of hydrofluoric acid to water =1:2, and removing residual metal titanium by using the prepared hydrofluoric acid solution; then, aqua regia is prepared according to the volume ratio of nitric acid to hydrochloric acid =1:3, and residual reactants on the surfaces of the diamond particles are removed through heating and soaking; and finally, washing the diamond particles by using deionized water until the washing liquid is neutral, and drying to obtain the diamond particles with etching pits on the surfaces, wherein the surface appearance of the obtained diamond is shown in figure 5.
Example 4
(1) Weighing 5g of diamond particles with the particle size of 40-45 meshes, ultrasonically cleaning the diamond particles in acetone for 30min to remove impurities on the surfaces of the diamond particles, then ultrasonically cleaning the diamond particles in deionized water, and drying the diamond particles for use;
(2) uniformly mixing the cleaned diamond particles and metal titanium powder (the particle size is 40-50 mu m) in a mass ratio of 1:2, putting the mixture into a ceramic crucible, then putting the ceramic crucible into a vacuum furnace, and starting heating after the vacuum degree is pumped to 5 x 10 < -3 > Pa. Heating to 750 deg.C at a heating rate of 10 deg.C/min, and maintaining for 10 min; then heating to 950 ℃ at the heating rate of 5 ℃/min, preserving the heat for 60min, and then cooling to room temperature along with the furnace;
(3) and (4) carrying out acid washing treatment on the heated product. Firstly, preparing a hydrofluoric acid solution according to the volume ratio of hydrofluoric acid to water =1:2, and removing residual metal titanium by using the prepared hydrofluoric acid solution; then, aqua regia is prepared according to the volume ratio of nitric acid to hydrochloric acid =1:3, and residual reactants on the surfaces of the diamond particles are removed through heating and soaking; and finally, washing the diamond particles by using deionized water until the washing liquid is neutral, and drying to obtain the diamond particles with etching pits on the surfaces, wherein the surface appearance of the obtained diamond is shown in figure 6.
Example 5
(1) Weighing 5g of diamond particles with the particle size of 40-45 meshes, ultrasonically cleaning the diamond particles in acetone for 30min to remove impurities on the surfaces of the diamond particles, then ultrasonically cleaning the diamond particles in deionized water, and drying the diamond particles for use;
(2) uniformly mixing the cleaned diamond particles and metal titanium powder (the particle size is 40-50 mu m) in a mass ratio of 1:2, putting the mixture into a ceramic crucible, then putting the ceramic crucible into a vacuum furnace, and pumping the vacuum degree to 5 x 10-3Heating was started after Pa. Heating to 750 deg.C at a heating rate of 10 deg.C/min, and maintaining for 10 min; then heating to 1000 ℃ at the heating rate of 5 ℃/min, preserving the heat for 60min, and then cooling to room temperature along with the furnace;
(3) and (4) carrying out acid washing treatment on the heated product. Firstly, preparing a hydrofluoric acid solution according to the volume ratio of hydrofluoric acid to water =1:2, and removing residual metal titanium by using the prepared hydrofluoric acid solution; then, aqua regia is prepared according to the volume ratio of nitric acid to hydrochloric acid =1:3, and residual reactants on the surfaces of the diamond particles are removed through heating and soaking; and finally, washing the diamond particles by using deionized water until the washing liquid is neutral, and drying to obtain the diamond particles with etching pits on the surfaces, wherein the surface appearance of the obtained diamond is shown in figure 7.
Experimental results verification example
The diamond morphology before treatment is shown in figure 2, and the diamond surface is smooth and has no defects. Fig. 3, 4, 5, 6 and 7 show the appearance of the diamond after etching treatment. Compared with the graph of fig. 2, after the etching treatment of the metal titanium powder is carried out on the graph of fig. 3, etching pits appear on the surface of the diamond, but due to the lower temperature, the etching pit traces on the surface of the diamond are shallower, the number of the etching pits is smaller, and the depth of the etching pits is shallower; in fig. 4, at higher temperatures, the diamond surface shows uniformly distributed etch pits, compared to fig. 3. The number and the depth of the etching pits are obviously increased; in comparison with fig. 4, fig. 5 and 6 show that the number of etching pits on the surface of the diamond is increased to a certain extent, and the quality ratio and the holding time have certain influence on the etching process, but the effect of no temperature is more obvious. In comparison with fig. 6, example 5 raised the final heating temperature to 1000 c, and it was found that the size and depth of the etch pits increased, but there was no significant increase in the number of etch pits.
In addition, through the analysis of the intermediate process of the five embodiments of the present invention, it is known from the XRD result that the original metal titanium powder and the diamond do not contain any impurity component, and when the mixture of the two is subjected to heat treatment at 850 ℃, and then cleaned with hydrofluoric acid, TiC exists on the surface of the diamond after etching, so the reaction principle of the present invention is different from that of the existing diamond etched by using metals such as iron, cobalt, nickel, etc., and the existing diamond etched by using metals such as iron, cobalt, nickel, etc. mainly forms the etching pits on the surface of the diamond due to the catalytic action of the metals such as iron, cobalt, nickel on the diamond, so that the diamond is graphitized first, and carbon atoms are diffused from graphite to metal, but the graphitization of the diamond causes the reduction of the diamond performance. In the invention, TiC is formed on the surface of the diamond, so that carbon atoms are lost on the surface of the diamond, and an etching pit is formed.
Meanwhile, as can be seen from the analysis of the results of the above examples, the rate of TiC formation increases with an increase in temperature.
Further, it is understood from the XPS results analysis of fig. 8 and 9 that after the removal of TiC from the diamond surface, the chemical composition of the etched diamond surface is not significantly changed from that of the original diamond surface.
FIG. 10 is a schematic view showing the relationship between the specific surface area of diamond and temperature, and it can be seen that the specific surface area of diamond increases with increasing temperature until reaching a maximum specific surface area of 0.31m at 1000 deg.C2·g-1Drawing (1) ofThe bending strength of the bending-resistant sample supported by the original diamond and the phenolic resin-based bonding agent after the titanium powder etching is given by 11, and it can be known that the bending strength of the diamond and the bonding agent after the titanium powder etching is increased along with the increase of the temperature, the bending strength of the diamond and the bonding agent after the etching treatment at 1000 ℃ is the maximum, the average bending strength is 59.4MPa, and the maximum bending strength of the diamond and the bonding agent after the titanium powder etching is improved by 56% compared with the bending strength of 38.1MPa of the original diamond and the bonding agent.
In conclusion, the diamond is etched by the metal titanium powder, so that obvious etching pits can be generated on the surface of the diamond, the specific surface area of diamond particles is increased, and meanwhile, the diamond particles are not graphitized and still have good strength. After the diamond is etched, the connection strength between the diamond particles and the bonding agent can be effectively enhanced, the self-sharpening performance of the diamond tool can be improved, the performance of the diamond tool is improved, and the service life of the diamond tool is prolonged.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (6)
1. A method for etching a surface of a synthetic diamond, comprising the steps of:
s1, uniformly mixing dried diamond particles and metal titanium powder with the particle size of 40-50 mu m in a mass ratio of 1: 1-1: 3, and then putting the mixture into a ceramic crucible;
s2, placing the ceramic crucible into a vacuum furnace, pumping the vacuum degree to 5.0 x 10 < -4 > Pa-5.0 x 10 < -3 > Pa, heating to 850-1000 ℃ at the heating rate of 5-10 ℃/min, preserving the temperature for 30-120 min, and cooling to room temperature along with the furnace;
and S3, treating the product obtained in the step S2 by using a hydrofluoric acid solution, then placing the product in aqua regia for heating and soaking, finally washing the product by using deionized water until the washing liquid is neutral, and drying the washing liquid to obtain the diamond particles with etching pits on the surfaces.
2. The method of claim 1, further comprising a step of pre-treating the diamond surface prior to S1.
3. A method of etching a synthetic diamond surface according to claim 2, wherein the step of pre-treating the diamond surface comprises: ultrasonically cleaning diamond particles with the particle size of 40-45 mu m in acetone for 30min, then ultrasonically cleaning in deionized water, and drying for S1.
4. The method for etching a surface of a synthetic diamond according to claim 1, wherein the step of heating the substrate to 850-1000 ℃ in S2 is performed by a step heating method.
5. The method of claim 4, wherein the segmented heating comprises a first segment heating process and a second segment heating process, wherein the first segment heating process comprises: heating to 750 ℃ at the heating rate of T1, and keeping the temperature for T1 time; and the second stage of heating process is to heat to 850-1000 ℃ at the temperature rising rate of T2, and to preserve heat for T2 time, wherein T1 is more than T2, and T1 is more than T2.
6. The method for etching a surface of a synthetic diamond according to claim 1, wherein the hydrofluoric acid solution used in S3 is a mixed solution of hydrofluoric acid and water at a volume ratio of 1: 2.
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Cited By (1)
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| CN114472882A (en) * | 2021-12-21 | 2022-05-13 | 山东昌润钻石股份有限公司 | Diamond surface directional etching method |
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