CN112473560B - Method for improving diamond conversion rate in production of polycrystalline diamond by explosion method - Google Patents
Method for improving diamond conversion rate in production of polycrystalline diamond by explosion method Download PDFInfo
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- CN112473560B CN112473560B CN202011387083.6A CN202011387083A CN112473560B CN 112473560 B CN112473560 B CN 112473560B CN 202011387083 A CN202011387083 A CN 202011387083A CN 112473560 B CN112473560 B CN 112473560B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/062—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies characterised by the composition of the materials to be processed
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/08—Application of shock waves for chemical reactions or for modifying the crystal structure of substances
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/0605—Composition of the material to be processed
- B01J2203/061—Graphite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2203/00—Processes utilising sub- or super atmospheric pressure
- B01J2203/06—High pressure synthesis
- B01J2203/065—Composition of the material produced
- B01J2203/0655—Diamond
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Abstract
The invention discloses a method for improving diamond conversion rate in polycrystalline diamond production by explosion method, which takes graphite asRaw materials, ni, cu, fe and Cr ions as additives, naOH as a neutralizer and H2SO4The preparation of the diamond production material is carried out for the activating agent, so that the conversion rate of the diamond is increased by 10-13%, the production cost is reduced, and the production efficiency is improved.
Description
Technical Field
The invention belongs to the technical field of diamond production equipment, and particularly relates to a method for improving diamond conversion rate in polycrystalline diamond production by an explosion method.
Background
Diamond is an ideal material for grinding and polishing due to the characteristic of 'hardest world', and because natural polycrystalline diamond (Carbonado type) has rare yield and high price, the diamond is generally manufactured by people at present. At present, the methods for artificially manufacturing diamond only comprise three methods, namely a static pressure method, a detonation method and an explosion method. The diamonds produced by the static pressure method are all single crystals, the grain diameter is usually between 1 and 600 mu m, and the method is suitable for manufacturing common diamond grinding wheels, common polishing abrasive materials and the like; the diamond produced by the detonation method is also single crystal, the average grain diameter is very small, usually about 12nm, the commercial dry powder aggregate grain size reaches 2 mu m, even a suspension prepared by a modifier and a surfactant has the coarsest aggregate grain size of 130-150 nm, the aggregate grain size distribution in the suspension is wide, and the diamond is mainly used as a lubricant at present; the diamond produced by the explosion method is polycrystalline diamond which is closest to natural carbonado diamond, and is suitable for grinding and polishing chips and hard disks.
At present, the method for explosion synthesis of diamond is to put graphite powder into a mould and press it into cylindrical (round or square or rectangular) graphite compact with the same shape as the flying piece in the explosion device. In order to adjust the density of the graphite compact, some graphite powders are added with metal powders such as iron, copper, cobalt and the like; in addition, the metal powder is added and simultaneously the cementing material such as resin is added, and the resin is removed by low-temperature (less than 300 ℃) sintering and the density of the graphite compact is improved. Then, the graphite compact is placed under the flyer of the explosive device, and a certain distance is ensured (the distance is the height). Detonate the detonator above the explosion device to explode the explosive column, push the flying piece to strike the graphite compact at a certain flying speed, and generate high temperature and high pressure in the graphite powder to cause transient phase change of the graphite. And finally, recovering the scattered graphite ash, screening and washing the graphite ash, and carrying out metal removal and residual graphite removal treatment by using strong acid such as nitric acid, sulfuric acid and the like and chemical agents such as strong oxidants and the like to obtain the synthesized diamond. Most of graphite raw materials for producing diamond in the prior art are graphite powder, or metal powder such as iron, copper, cobalt and the like is added into the graphite powder, the diamond conversion rate cannot be changed by adopting all the raw materials, and the problem of low diamond conversion rate still exists.
Therefore, there is an urgent need to develop a method for increasing the diamond conversion rate in the explosive process of producing polycrystalline diamond to solve the above problems.
Disclosure of Invention
In order to solve the problems of the background art, the present invention provides a method for increasing the diamond conversion rate in the explosive process of producing polycrystalline diamond.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for increasing diamond conversion in explosive process polycrystalline diamond production comprising the steps of:
s1, taking graphite as a raw material, taking Ni, cu, fe and Cr ions as additives, naOH as a neutralizer and H2SO4 as an activator;
s2, firstly dissolving salts corresponding to Ni, cu, fe and Cr ions in one barrel, and dissolving NaOH in the other barrel for later use;
s3, putting graphite into a reaction kettle, adding water, setting the weight of the water to be 3 times that of the graphite at 60 ℃, opening a heating switch of the reaction kettle, and uniformly stirring;
s4, slowly adding 98% H into the reaction kettle2SO4Solution of H2SO4The weight of the solution is 2% of the weight of the graphite;
s5, slowly adding the prepared solution containing Ni, cu, fe and Cr ions into a reaction kettle, wherein the weight of the metal salt containing the Ni, cu, fe and Cr ions is 10-40% of that of the graphite;
s6, reacting the materials in a reaction kettle at the temperature of 60 ℃, and continuously stirring for 90 minutes;
s7, adding a NaOH solution into the stirred material, wherein the weight of NaOH is 10% of that of the graphite;
s8, continuing to stir for 30 minutes, and stopping heating;
s9, adding water, stopping stirring, and waiting for the materials to precipitate;
s10, pouring settled upper-layer water into a neutralization pond, and repeating for multiple times until the water is neutral;
s11, placing the neutralized materials into a centrifugal machine for dehydration;
s12, placing the dehydrated materials into a tray, placing the tray into an oven, baking for 24 hours at the temperature of 120 ℃, and drying the materials;
s13, putting the dried materials into a graphite pot, putting the graphite pot into a sintering furnace with protective gas for heating, and finally cooling for later use;
and S14, adopting the standby material as a graphite raw material for producing the diamond, and adding the graphite raw material into an explosion device for producing the diamond.
Preferably, in step S13, the temperature profile of the sintering furnace is set in the order of:
the temperature is raised to 6 ℃ per minute and is raised to 350 ℃ within 55 minutes; preserving the heat for 1 hour;
the temperature is raised to 6 ℃ per minute and is raised to 750 ℃ within 67 minutes; preserving the heat for 1 hour;
the temperature is raised to 6 ℃ per minute and is raised to 950 ℃ within 33 minutes; after preserving heat for 3 hours, cutting off the power of the sintering furnace, and naturally cooling;
and when the temperature is lower than 150 ℃, opening the furnace door, taking out the materials, and cooling to room temperature for later use.
Preferably, in step S13, the shielding gas is nitrogen.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes graphite as raw material, ni, cu, fe and Cr ions as additives, naOH as neutralizer and H2SO4The preparation of the diamond production material is carried out for the activating agent, so that the conversion rate of the diamond is increased by 10-13%, the production cost is reduced, and the production efficiency is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides the following technical scheme:
a method for increasing diamond conversion in explosive process polycrystalline diamond production comprising the steps of:
s1, taking graphite as a raw material, taking Ni, cu, fe and Cr ions as additives, naOH as a neutralizer and H2SO4 as an activator;
s2, firstly dissolving salts corresponding to Ni, cu, fe and Cr ions in one barrel, and dissolving NaOH in the other barrel for later use;
s3, putting graphite into a reaction kettle, adding water, setting the weight of the water to be 3 times that of the graphite at 60 ℃, opening a heating switch of the reaction kettle, and uniformly stirring;
s4, slowly adding 98% H into the reaction kettle2SO4Solution of H2SO4The weight of the solution is 2% of the weight of the graphite;
s5, slowly adding the prepared solution containing Ni, cu, fe and Cr ions into a reaction kettle, wherein the weight of the metal salt containing the Ni, cu, fe and Cr ions is 10-40% of that of the graphite;
s6, reacting the materials in a reaction kettle at the temperature of 60 ℃, and continuously stirring for 90 minutes;
s7, adding a NaOH solution into the stirred material, wherein the weight of NaOH is 10% of that of the graphite;
s8, continuing to stir for 30 minutes, and stopping heating;
s9, adding water, stopping stirring, and waiting for the materials to precipitate;
s10, pouring settled upper-layer water into a neutralization pond, and repeating for multiple times until the water is neutral;
s11, placing the neutralized materials into a centrifugal machine for dehydration;
s12, placing the dehydrated materials into a tray, placing the tray into an oven, baking for 24 hours at the temperature of 120 ℃, and drying the materials;
s13, putting the dried material into a graphite pot, putting the graphite pot into a sintering furnace with protective gas for heating, and finally cooling for later use;
and S14, adopting the standby material as a graphite raw material for producing the diamond, and adding the graphite raw material into an explosion device for producing the diamond.
Preferably, in step S13, the temperature profile of the sintering furnace is set in the order of:
the temperature is raised to 6 ℃ per minute and is raised to 350 ℃ within 55 minutes; preserving the heat for 1 hour;
the temperature is raised to 6 ℃ per minute and is raised to 750 ℃ within 67 minutes; preserving the heat for 1 hour;
the temperature is raised to 6 ℃ per minute and is raised to 950 ℃ within 33 minutes; after preserving heat for 3 hours, cutting off the power of the sintering furnace, and naturally cooling;
and when the temperature is lower than 150 ℃, opening the furnace door, taking out the materials, and cooling to room temperature for later use.
Preferably, in step S13, the shielding gas is nitrogen.
One specific example is given below:
a method of increasing diamond conversion in the explosive production of polycrystalline diamond comprising the steps of:
s1, taking graphite (generally adopting flake graphite and earthy graphite) as raw materials, fe ions as an additive, naOH as a neutralizer and H2SO4Is an activating agent;
s2, dissolving FeCl in a plastic barrel3.6H2Dissolving NaOH in another plastic barrel for later use;
s3, putting graphite into an enamel reaction kettle, adding water, setting the weight of the water to be 3 times that of the graphite at 60 ℃, opening a heating switch of the reaction kettle, and uniformly stirring;
s4, slowly adding 98% H into the enamel reaction kettle2SO4Solution of H2SO4The weight of the solution is 2% of the weight of the graphite;
s5, preparing FeCl3.6H2Slowly adding O solution into enamel reactor and FeCl3.6H2The weight of O is 20 percent of the weight of graphite;
s6, reacting the materials in an enamel reaction kettle at the temperature of 60 ℃, and continuously stirring for 90 minutes;
s7, adding a NaOH solution into the stirred material, wherein the weight of NaOH is 10% of that of the graphite;
s8, continuing to stir for 30 minutes, and stopping heating;
s9, adding water, stopping stirring, and waiting for the materials to precipitate;
s10, pouring settled upper-layer water into a neutralization pond, and repeating for multiple times until the water is neutral;
s11, placing the neutralized materials into a centrifugal machine for dehydration;
s12, placing the dehydrated materials into a tray, placing the tray into an oven, baking for 24 hours at the temperature of 120 ℃, and drying the materials;
s13, putting the dried materials into a graphite pot, putting the graphite pot into a sintering furnace with nitrogen for heating, and sequentially setting the temperature curves of the sintering furnace as follows:
the temperature is raised to 6 ℃ per minute and is raised to 350 ℃ within 55 minutes; preserving the heat for 1 hour;
the temperature is raised to 6 ℃ per minute and is raised to 750 ℃ within 67 minutes; preserving the heat for 1 hour;
the temperature is raised to 6 ℃ per minute and is raised to 950 ℃ within 33 minutes; after preserving heat for 3 hours, cutting off the power of the sintering furnace, and naturally cooling;
and when the temperature is lower than 150 ℃, opening the furnace door, taking out the materials, and cooling to room temperature for later use.
And S14, adopting the standby material as a graphite raw material for producing the diamond, and adding the graphite raw material into an explosion device for producing the diamond.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (3)
1. A method for increasing the diamond conversion rate in the explosive process of producing polycrystalline diamond, comprising the steps of:
s1, taking graphite as a raw material, ni, cu, fe and Cr ions as additives, naOH as a neutralizing agent and H2SO4Is an activating agent;
s2, firstly dissolving salts corresponding to Ni, cu, fe and Cr ions in one barrel, and dissolving NaOH in the other barrel for later use;
s3, putting graphite into a reaction kettle, adding water, setting the weight of the water to be 3 times that of the graphite at 60 ℃, opening a heating switch of the reaction kettle, and uniformly stirring;
s4, slowly adding 98% H into the reaction kettle2SO4Solution of H2SO4The weight of the solution is 2% of the weight of the graphite;
s5, slowly adding the prepared solution containing Ni, cu, fe and Cr ions into a reaction kettle, wherein the weight of the metal salt containing the Ni, cu, fe and Cr ions is 10-40% of that of the graphite;
s6, reacting the materials in a reaction kettle at the temperature of 60 ℃, and continuously stirring for 90 minutes;
s7, adding a NaOH solution into the stirred material, wherein the weight of NaOH is 10% of that of the graphite;
s8, continuing to stir for 30 minutes, and stopping heating;
s9, adding water, stopping stirring, and waiting for the materials to precipitate;
s10, pouring settled upper-layer water into a neutralization pond, and repeating for multiple times until the water is neutral;
s11, placing the neutralized materials into a centrifugal machine for dehydration;
s12, placing the dehydrated materials into a tray, placing the tray into an oven, baking for 24 hours at the temperature of 120 ℃, and drying the materials;
s13, putting the dried material into a graphite pot, putting the graphite pot into a sintering furnace with protective gas for heating, and finally cooling for later use;
and S14, adopting the standby material as a graphite raw material for producing the diamond, and adding the graphite raw material into an explosion device for producing the diamond.
2. The method for increasing the diamond conversion rate in explosive production of polycrystalline diamond according to claim 1, wherein in step S13, the temperature profile of the sintering furnace is set in the order of:
the temperature is raised to 6 ℃ per minute and is raised to 350 ℃ within 55 minutes; preserving the heat for 1 hour;
the temperature is raised to 6 ℃ per minute and is raised to 750 ℃ within 67 minutes; preserving the heat for 1 hour;
the temperature is raised to 6 ℃ per minute and is raised to 950 ℃ within 33 minutes; after preserving heat for 3 hours, cutting off the power of the sintering furnace, and naturally cooling;
and when the temperature is lower than 150 ℃, opening the furnace door, taking out the materials, and cooling to room temperature for later use.
3. The method for increasing diamond conversion in explosive production of polycrystalline diamond according to claim 1, wherein the shielding gas is nitrogen in step S13.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN85106775A (en) * | 1985-09-07 | 1986-07-02 | 哈尔滨电碳研究所 | Graphite for diamond synthesis and manufacture method thereof |
| JPH06121923A (en) * | 1992-10-12 | 1994-05-06 | Mitsui Mining Co Ltd | Production of diamond |
| CN1047324C (en) * | 1993-11-27 | 1999-12-15 | 大连理工大学 | Expansion graphite method for explosion synthesis of diamond |
| CN1273378C (en) * | 2004-01-21 | 2006-09-06 | 岳敏 | Method for manufacturing expanded graphite with ultra-low microelement |
| CN102631922B (en) * | 2012-03-28 | 2015-04-08 | 长沙星城微晶石墨有限公司 | Method for preparing metallic cladding expansion graphite |
| CN105883780B (en) * | 2015-12-15 | 2017-12-05 | 中南大学 | A kind of method for preparing high-purity crystalline flake graphite |
| CN105483824A (en) * | 2016-01-11 | 2016-04-13 | 信阳师范学院 | Method for preparing monocrystal double-layer graphene |
| CN107337203B (en) * | 2017-08-31 | 2020-09-01 | 鸡西市东北亚矿产资源有限公司 | Method for preparing high-purity graphite |
| CN108163850B (en) * | 2017-12-22 | 2021-07-13 | 郑州中南杰特超硬材料有限公司 | Preparation method of carbon source for synthesizing large-scale polycrystalline diamond |
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