CN111809227A - Method for preparing porous monocrystalline diamond - Google Patents
Method for preparing porous monocrystalline diamond Download PDFInfo
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- CN111809227A CN111809227A CN202010526340.3A CN202010526340A CN111809227A CN 111809227 A CN111809227 A CN 111809227A CN 202010526340 A CN202010526340 A CN 202010526340A CN 111809227 A CN111809227 A CN 111809227A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/12—Single-crystal growth directly from the solid state by pressure treatment during the growth
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B30/00—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
- C30B30/06—Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using mechanical vibrations
Abstract
The method for preparing the porous monocrystalline diamond comprises the steps of taking a diamond seed crystal as a growth substrate, wrapping the diamond seed crystal with a mixture of diamond powder crystals and metal catalyst powder, sealing and forming, carrying out oriented adhesion growth by taking the diamond seed crystal as the substrate through adjusting the crystal orientation in a molten catalyst environment under the condition of high temperature and high pressure in a diamond stable region, reducing the temperature and pressure conditions required by crystal growth by using the metal catalyst, providing a proper environment for oriented adhesion of the diamond powder crystals, and increasing the growth rate of the diamond. Along with the growth of the diamond seed crystal, because the growth rate is high, gaps and other defects exist among the diamond powder crystals and at the attachment and joint part of the diamond powder crystals and the seed crystal substrate, after the seed crystal grows up, the diamond powder crystals and the metal catalyst which do not participate in the growth are removed through acid washing and vibration impact, and then the porous monocrystalline diamond is obtained.
Description
Technical Field
The invention belongs to the technical field of crystal growth, and particularly relates to a method for preparing porous single crystal diamond, in particular to a method for synthesizing large porous diamond single crystal.
Background
The synthesis of diamond is usually to add catalyst into graphite under high temperature and high pressure to convert it into diamond, and the current method for synthesizing large single crystals of diamond commonly used in the field of high temperature and high pressure is as follows: temperature gradient methods and thin film growth methods.
For the synthesis of porous diamond, k.honda et al in japan prepared nanoporous honeycomb diamond by a plasma etching method, but the synthesized diamond was a thin film and the pore diameter was only 400 nm; czech
Varga et al grow porous diamond films of various shapes by CVD, but only thin films and small size; russian AlekseChepurov et al used etching of synthetic single crystal diamond with iron nanoparticles in a hydrogen atmosphere to obtain pore sizes: 0.5-0.7 μm, individual pore depth: 3 μm porous diamond.
The porous diamond synthesized by the method is a small porous diamond film layer, has low strength and small thickness, and is not suitable for wide application.
Disclosure of Invention
In view of the above problems, it is an object of the present invention to provide a method for producing porous single-crystal diamond.
In order to achieve the above purpose, the invention adopts the technical scheme that: a method of making porous single crystal diamond comprising the steps of:
and 3, removing diamond particles and metal catalyst particles which do not participate in growth in the diamond compact by adopting acid washing and vibration impact to obtain the porous monocrystalline diamond.
The method comprises the steps of taking a diamond seed crystal as a growth substrate, wrapping the diamond seed crystal with a mixture of diamond powder crystals and metal catalyst powder, sealing and wrapping, taking the diamond seed crystal as the substrate for growth of the diamond powder crystals under the high-temperature and high-pressure condition of a diamond growth stable area, and adjusting the grain orientation of the diamond powder crystals to realize directional adhesion with the diamond seed crystal under the action of the catalyst so as to achieve the same grain orientation. The metal catalyst reduces the temperature and pressure conditions required by crystal growth, provides a proper environment for the directional adhesion of diamond powder crystals, and increases the growth rate of diamond. Along with the growth of the diamond seed crystal, because the growth rate is high, gaps and other defects exist among the diamond powder crystals and at the attachment and joint part of the diamond powder crystals and the seed crystal substrate, after the seed crystal grows up, the diamond powder crystals and the metal catalyst which do not participate in the growth are removed through acid washing and vibration impact, and then the porous monocrystalline diamond is obtained. The grain size of the prepared porous monocrystalline diamond is influenced by the grain size of the diamond seed crystal, the temperature and pressure condition and the high-temperature and high-pressure treatment time, the larger the grain size of the diamond seed crystal is, the longer the high-temperature and high-pressure treatment time is, the larger the grain size of the prepared porous monocrystalline diamond is, porous monocrystalline diamonds with different sizes can be prepared according to the requirements, the porous monocrystalline diamond with large size can be used for preparing cutters, and the porous monocrystalline diamond with small size can be used for preparing adsorbents and abrasives. When the tool is manufactured into the tool, due to the porous characteristic, the self-sharpening performance of the tool is enhanced, the holding force of the diamond and the tool handle substrate is enhanced, and therefore the attaching force and the cutting performance of the tool and the tool handle are improved. When the porous diamond is used as an adsorbing material, an electrode material and the like, the porous diamond has a higher specific surface area and a larger contact area with the material, so that the adsorption performance and the electrolysis efficiency are greatly improved.
Specifically, in the step 1, the diamond seed crystal, the diamond powder crystal and the metal catalyst powder are mixed and then placed in a die for prepressing and forming to obtain a massive sample, sealing and packaging are performed to obtain a sealing block, the prepressing and blocking are convenient for sealing and packaging, meanwhile, oxygen in raw material particles is removed, and raw material oxidation in the step 2 is avoided.
Specifically, in the step 1, the block-shaped sample is subjected to hydrogen reduction at 300-1200 ℃ and then is hermetically wrapped, and the hydrogen reduction is performed to further remove oxygen in the sample, so that the raw material is not oxidized by oxygen in the sintering process in the step 2.
Specifically, in the step 1, the diamond seed crystal is a single crystal diamond block with a grain size of more than 100 μm, the grain size of the diamond powder crystal is preferably 3 nm-10 μm, the diamond seed crystal size can be selected to be larger in order to prepare a large porous diamond single crystal with a larger size, but due to the difference of interface energy, the larger the difference of specific surface area between the diamond seed crystal and the diamond microcrystal in the grain size range is, the better the difference is, the size of the diamond powder crystal should be smaller, the grain size of the diamond seed crystal is kept about 1 μm, and the ratio of the grain size of the diamond seed crystal to the grain size of the diamond powder crystal is (10-1000): 1. If the match is not reasonable, for example: selecting 1cm diamond seed crystal and 1nm diamond powder crystal, wherein the difference between the specific surface areas of the two is too large, and the diamond powder crystal can form a core by itself and cannot grow; the metal catalyst powder is at least one of iron powder, cobalt powder, nickel powder and alloy powder thereof, such as iron-nickel alloy powder. Specifically, in the step 1, the diamond powder crystal and the metal catalyst powder are mixed according to the volume/weight ratio of 1 (1-10), the ratio can grow in a certain range, if the ratio is too small, the diamond powder crystal is completely fused into the catalyst and cannot grow, if the ratio is too large, the diamond powder crystal is agglomerated or abnormally grown, and the diamond powder crystal cannot be attached to and grow on the surface of the seed crystal.
Specifically, the sample is hermetically wrapped in an assembly block in the step 1, the assembly block comprises a magnesium oxide cavity, a carbon tube, a dolomite tube and a pyrophyllite block which are sequentially sleeved from inside to outside, wherein the upper end and the lower end of the dolomite tube are respectively provided with a dolomite ring and a molybdenum sheet from inside to outside, the upper end and the lower end of the pyrophyllite block are respectively provided with a through hole which are coaxial with the dolomite tube, a steel plug is arranged in the through hole and abutted against the molybdenum sheet, the upper end and the lower end of the carbon tube are respectively provided with a carbon sheet, the inner ring of the dolomite ring is provided with a carbon column, the two ends of the carbon column are respectively abutted against the molybdenum sheet and the carbon sheet, and the diamond seed crystal, diamond powder crystal and metal catalyst powder are mixed and then hermetically wrapped in the magnesium oxide cavity; and 2, placing the assembled assembly block in a cubic press for high-temperature and high-pressure treatment, starting the press, extruding six surfaces of the pyrophyllite block by six top hammers of the press, so that high pressure is generated at a sample in the magnesium oxide cavity, electrifying the upper top hammer and the lower top hammer of the press, and generating high temperature in the assembly block.
Specifically, in the step 2, the sealing block is treated for 10 minutes or more under the conditions of 5.2-8 GPa and 1200-1600 ℃.
Specifically, the step 3 of performing acid washing on the diamond compact specifically comprises the following steps: cleaning in hot dilute nitric acid for a long time, soaking in aqua regia, dissolving metal catalyst in acid washing solution, and removing impurities by ultrasonic vibration.
The invention has the beneficial effects that:
the method comprises the steps of taking a diamond seed crystal as a growth substrate, wrapping the diamond seed crystal with a mixture of diamond powder crystals and metal catalyst powder, sealing and wrapping, taking the diamond seed crystal as the substrate for growth of the diamond powder crystals under the high-temperature and high-pressure condition of a diamond growth stable area, and adjusting the grain orientation of the diamond powder crystals to realize directional adhesion with the diamond seed crystal under the action of the catalyst so as to achieve the same grain orientation. The metal catalyst reduces the temperature and pressure conditions required by crystal growth, provides a proper environment for the directional adhesion of diamond powder crystals, and increases the growth rate of diamond. Along with the growth of the diamond seed crystal, because the growth rate is high, gaps and other defects exist among the diamond powder crystals and at the attachment and joint part of the diamond powder crystals and the seed crystal substrate, after the seed crystal grows up, the diamond powder crystals and the metal catalyst which do not participate in the growth are removed through acid washing and vibration impact, and then the porous monocrystalline diamond is obtained.
Drawings
FIG. 1 is an assembly view adopted in the embodiment;
FIG. 2 is a general view of a porous single crystal diamond mass obtained in example 1;
FIG. 3 is a partial view of an SEM test of a porous single crystal diamond mass obtained in example 1;
FIG. 4 is a Raman detection spectrum of the porous diamond single crystal obtained in example 1;
FIG. 5 is a Laue diffraction pattern of the porous diamond single crystal obtained in example 1;
FIG. 6 is an SEM test chart of the porous single crystal diamond mass obtained in example 2;
FIG. 7 is an SEM test chart of the porous single crystal diamond mass obtained in example 3;
FIG. 8 is an SEM test chart of the porous single crystal diamond mass obtained in example 4;
FIG. 9 is an SEM test chart of the porous single crystal diamond mass obtained in example 5;
wherein, 1 is a magnesium oxide cavity, 2 is a carbon tube, 3 is a dolomite tube, 4 is a pyrophyllite block, 5 is a dolomite ring, 6 is a molybdenum sheet, 7 is a steel plug, 8 is a carbon sheet, 9 is a carbon column, 10 is a block sample, 11 is, 12 is.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1
The present embodiment provides a method of preparing porous single crystal diamond, comprising the steps of:
and 3, cleaning the diamond compact in dilute nitric acid, then soaking and cleaning the diamond compact in aqua regia to remove diamond powder crystals and metal catalyst powder which do not participate in growth, and finally carrying out ultrasonic cleaning to obtain the porous monocrystalline diamond.
The porous single crystal diamond obtained in the embodiment is subjected to SEM scanning electron microscope test, and the test result is shown in FIGS. 2 and 3, wherein the size of the obtained porous single crystal diamond is about 683 micrometers; performing Raman test, wherein the test result is shown in figure 4, the initial line represents the Raman peak of the artificial single crystal diamond sample, the convex line represents the Raman peak on the surface of the porous single crystal diamond, the concave line represents the Raman peak at the pore of the porous single crystal diamond, and Raman spectra corresponding to the diamond material can be obtained on the surface of the porous single crystal diamond and the material at the pore, so that no other impurities grow on the sample; from the Laue diffraction pattern shown in FIG. 5, it is a single crystal sample.
Example 2
This embodiment is different from embodiment 1 in that: the grain size of the synthetic single crystal diamond used in step 1 was 620 μm, and the synthetic single crystal diamond was sintered at 5.5GPa and 1260 ℃ for 30 minutes in step 2, and the other operations were the same as in example 1.
The porous single crystal diamond obtained in this example was subjected to SEM scanning electron microscope test, and the test result is shown in fig. 6, and the size of the obtained porous single crystal diamond was about 660 μm.
Example 3
This embodiment is different from embodiment 1 in that: the grain size of the synthetic single crystal diamond used in step 1 was 625 μm, and the synthetic single crystal diamond was sintered at 5.5GPa and 1260 ℃ for 15 minutes in step 2, and the other operations were the same as in example 1.
The porous single-crystal diamond obtained in this example was subjected to SEM scanning electron microscope test, and the test result is shown in fig. 7, and the size of the obtained porous single-crystal diamond was about 650 μm.
Example 4
The present embodiment provides a method of preparing porous single crystal diamond, comprising the steps of:
and 3, cleaning the diamond compact in dilute nitric acid, then soaking and cleaning the diamond compact in aqua regia to remove diamond powder crystals and metal catalyst powder which do not participate in growth, and finally carrying out ultrasonic cleaning to obtain the porous monocrystalline diamond.
The porous single crystal diamond obtained in this example was subjected to SEM scanning electron microscope test, and the test result is shown in fig. 8, where the size of the obtained porous single crystal diamond was about 680 μm.
Example 5
The present embodiment provides a method of preparing porous single crystal diamond, comprising the steps of:
and 3, cleaning the diamond compact in dilute nitric acid, then soaking and cleaning the diamond compact in aqua regia to remove diamond powder crystals and metal catalyst powder which do not participate in growth, and finally carrying out ultrasonic cleaning to obtain the porous monocrystalline diamond.
The porous single crystal diamond obtained in this example was subjected to SEM scanning electron microscopy, and the test result is shown in fig. 9, where the size of the obtained porous single crystal diamond was about 660 μm.
The above examples 1 to 5, in conjunction with fig. 2 to 9, show that the method provided by the present invention can be used to repeatedly produce porous single crystal diamond, and the method has the advantages of no obvious defects in the quality of the synthesized crystal, irregular shape, high porosity, large specific surface area, simple operation, low cost, repeatability, and capability of meeting the requirements of mass production and the requirements of some fields on porous diamond; comparing fig. 2, 3, 6, 7, 8, and 9, it can be seen that the pores of the porous single crystal diamonds obtained in examples 1 to 3 and 4 to 5 decrease progressively, respectively, indicating that the longer the sintering time under the same temperature and pressure conditions, the more pores of the porous single crystal diamonds are sintered, and that the higher the temperature and pressure conditions, the more pores of the porous single crystal diamonds are sintered under the same sintering time conditions.
The above examples of the present invention are merely illustrative of the present invention and are not intended to limit the embodiments of the present invention. Variations and modifications in other variations will occur to those skilled in the art upon reading the foregoing description. Not all embodiments are exhaustive. All obvious changes and modifications of the present invention are within the scope of the present invention.
Claims (9)
1. A method of making porous single crystal diamond comprising the steps of:
step 1, sealing and wrapping a sample obtained by mixing diamond seed crystals, diamond powder crystals and metal catalyst powder to obtain a sealing block;
step 2, processing the sealing block under the conditions of 5.2-8 GPa and high temperature and high pressure of 1200-1600 ℃, and removing the sealing package to obtain a diamond compact;
and 3, removing diamond powder crystals and metal catalyst powder which do not participate in growth in the diamond compact by adopting acid washing and vibration impact to obtain the porous monocrystalline diamond.
2. The method for preparing porous monocrystalline diamond according to claim 1, wherein in the step 1, the diamond seed crystal, the diamond powder crystal and the metal catalyst powder are mixed and then placed in a mold for prepressing forming to obtain a block sample, and then the block sample is sealed and wrapped to obtain a sealing block.
3. The method for preparing porous single-crystal diamond according to claim 2, wherein in the step 1, the block sample is subjected to hydrogen reduction at 300-1200 ℃ and then is hermetically wrapped.
4. The method for preparing porous single-crystal diamond according to claim 1, wherein the diamond seed crystal in step 1 is a single-crystal diamond particle body having a grain size of 100 μm or more, the diamond powder crystal has a grain size of 3nm to 10 μm, and the metal catalyst powder is at least one of iron powder, cobalt powder, and nickel powder.
5. The method for producing porous single-crystal diamond according to claim 1 or 4, wherein the ratio of the grain size of the diamond seed crystal to the grain size of the diamond powder crystal is (10-1000): 1.
6. The method for preparing porous single-crystal diamond according to claim 1 or 4, wherein the diamond powder crystal and the metal catalyst powder are mixed in a volume/weight ratio of 1 (1-10) in the step 1.
7. The method for preparing porous single-crystal diamond according to claim 1, wherein the sample is hermetically wrapped in an assembly block in step 1, the assembly block comprises a magnesium oxide cavity, a carbon tube, a dolomite tube and a pyrophyllite block which are sequentially sleeved from inside to outside, wherein a dolomite ring and a molybdenum sheet are sequentially arranged at the upper end and the lower end of the dolomite tube from inside to outside respectively, through holes coaxial with the dolomite tube are respectively arranged at the upper end and the lower end of the pyrophyllite block, a steel plug is arranged in each through hole and abutted against the molybdenum sheet, carbon sheets are respectively arranged at the upper end and the lower end of the carbon tube, a carbon column is arranged on the inner ring of the dolomite ring, two ends of the carbon column are abutted against the molybdenum sheet and the carbon sheet respectively, and a diamond seed crystal, a diamond powder crystal and a metal catalyst powder are mixed and then hermetically wrapped in the magnesium oxide cavity; and in the step 2, the assembled assembly block is placed in a cubic press for high-temperature and high-pressure treatment.
8. The method for producing a porous single crystal diamond according to claim 1, wherein the sealing block is treated at 5.2 to 8GPa for a period of 10 minutes or more at 1200 to 1600 ℃ in step 2.
9. The method for preparing porous single crystal diamond according to claim 1, wherein the step 3 of acid-washing the diamond compact is specifically: washing in dilute nitric acid, and soaking in aqua regia.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112892411A (en) * | 2021-01-25 | 2021-06-04 | 四川大学 | Method for growing large-particle diamond at high temperature and high pressure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112892411A (en) * | 2021-01-25 | 2021-06-04 | 四川大学 | Method for growing large-particle diamond at high temperature and high pressure |
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