CN102557024A - Reduction method of composite material particles of graphite for synthetic diamond and contact agent - Google Patents
Reduction method of composite material particles of graphite for synthetic diamond and contact agent Download PDFInfo
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- CN102557024A CN102557024A CN2011104289553A CN201110428955A CN102557024A CN 102557024 A CN102557024 A CN 102557024A CN 2011104289553 A CN2011104289553 A CN 2011104289553A CN 201110428955 A CN201110428955 A CN 201110428955A CN 102557024 A CN102557024 A CN 102557024A
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- graphite
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- material granular
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Abstract
The invention discloses a reduction method of composite material particles of graphite for a synthetic diamond and a contact agent. The method comprises the following processing steps of: placing the composite material particles of the graphite and the contact agent into a microwave kiln, introducing inert gas firstly to evacuate air in the microwave kiln, then introducing H2, wherein the volume ratio of the H2 to the inert gas is 2%-10%, heating to achieve 1050-1100 DEG C by utilizing microwaves under the mixed atmosphere of the H2 and the inert gas, maintaining the highest temperature for 30-60min, finally, cooling to be below 60 DEG C to discharge, and performing packaging in a sealing manner after discharging. In the reduction method, the microwaves are utilized to heat the composite material particles of the graphite and the contact agent to perform roasting reduction, the roasting reduction time through heating is reduced, the production efficiency of a product is remarkably improved, the technical process is shortened, the energy source is saved, and furthermore, the composite material particles of the graphite and the contact agent are heated uniformly during heating roasting reduction, and the product quality is good. The amount of introduced H2 is 2-10%, the expense of reducing gas can be greatly reduced and the potential safety hazards of equipment can be eliminated.
Description
Technical field
The present invention relates to the method for reducing of a kind of graphite and catalyst composite material granular, particularly relate to the method for reducing of a kind of graphite for diamond synthesis and catalyst composite material granular.
Background technology
Graphite and catalyst composite material granular often adopt conventional electrically heated reductive technology in traditional man-made diamond industry, and this technological process exists following not enough:
1, equipment requirements at first vacuumizes, and vacuum system is damaged easily, and there is potential safety hazard in equipment.
2, the roasting reduction process feeds pure hydrogen, and reducing gas (hydrogen) consumption is big, and expense is higher, and potential safety hazard is big.
3, conventional electrically heated heat energy is passed to material surface through convection current, conduction or radiating mode, again by surface conductance to material internal, until reaching thermal equilibrium.During this period, can not be the completely adiabatic sealing of heating environment, and for the structural state that makes material internal with surperficial identical; Reach the purpose of grilling thoroughly, the time of heat tracing generally all can be very long, and a large amount of heats are easy to be lost in the environment and go; Thereby cause great power loss, simultaneously, because the heat tracing time is longer; Required shielding gas large usage quantity has not only increased production cost, and has caused the pollution of environment.
Summary of the invention
It is short that technical problem to be solved by this invention provides a kind of heating roasting reduction time, and production efficiency is high, and capacity usage ratio is high, reduces environmental pollution, the method for reducing of graphite for diamond synthesis that production cost is low and catalyst composite material granular.
In order to solve the problems of the technologies described above; The method of reducing of graphite for diamond synthesis provided by the invention and catalyst composite material granular; Comprise following process step: graphite and catalyst composite material granular are put into microwave kiln; Elder generation feeds rare gas element and gets rid of the air in the microwave kiln, and feeding and rare gas element volume ratio are 2%～10% H again
2, at rare gas element and H
2Mixed atmosphere in utilize microwave heating to be rapidly heated to 1050～1100 ℃, at top temperature place insulation 30～60min, be cooled to 60 ℃ at last then with bottom discharge, pack immediately after the discharging.
Say that in more detail said rare gas element is nitrogen or argon gas; The total feeding amount of described mixed gas and the relation of graphite and catalyst composite material granular are 0.50～0.75m
3/ kg.
Adopt the graphite for diamond synthesis of technique scheme and the method for reducing of catalyst composite material granular, utilize microwave heating that graphite and catalyst composite material granular are carried out reducing roasting, feed H
2Volume only account for 2%～10% of mixed gas.Microwave heating technique is to utilize the basic fine structure coupling of special wave band that microwave has and material and produce heat, and the dielectric loss of material in EM field makes its integral body be heated to the method that temperature raises.Because microwave has stronger penetrativity, can be deep into the inside of sample, so; Utilization microwave heating roasting reduction can make inside and outside graphite and the catalyst composite material granular equably the overall absorption micro-wave energy and be heated, and it is different fully that its inner thermal gradient and direction of heat flow and routine heat, and can realize rapid and uniform heating and can not cause that sample heats reducing roasting inhomogeneous; Simultaneously, microwave almost can form instant heating to graphite and catalyst composite material granular, so can reduce the heating roasting reduction time greatly; Significantly improve production efficiency of products, reduce the production cycle, and micro-wave energy can directly be absorbed by material; Capacity usage ratio is very high; In addition, because the heating roasting reduction time is short, the shielding gas that expends in the roasting reduction process and the consumption of reducing gas also reduce greatly; Reduce unnecessary environmental pollution, practiced thrift production cost simultaneously.
In sum; The present invention utilizes microwave heating that graphite and catalyst composite material granular are carried out roasting reduction, has reduced the heating roasting reduction time, significantly improves production efficiency of products; Shorten technological process; Save energy, and graphite and catalyst composite material granular are heated evenly in heating roasting reduction process, and product quality is better; Simultaneously, feed H
2Amount be 2%～10%, can reduce the expense of reducing gas significantly, eliminated device security hidden danger.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
The present invention is done the explanation of further detail below in conjunction with accompanying drawing and instance.
Embodiment 1:
At first in the microwave burner hearth that installs graphite and catalyst composite material granular sample, feed nitrogen; In order to get rid of the air in the microwave burner hearth; In heating roasting reduction process, feeding volume is the mixed gas of 8% hydrogen and 92% nitrogen, and the total feeding amount of mixed gas and the relation of graphite and catalyst composite material granular are 0.70m
3/ kg rapid heating is warming up to 1060 ℃, and 1060 ℃ of insulation 60min under the mixed gas of 8% hydrogen and 92% nitrogen are cooled to 50 ℃ with bottom discharge again, and then that roasting is good catalyst composite material granular packs.
The present invention compares with traditional conventional electric heating roasting reducing process, but saves energy 40%, and the oxygen level of graphite and catalyst composite material granular increased the catalytic effect of catalyst less than 80ppm, improved the output and the quality of diamond synthesis.
Embodiment 2:
At first in the microwave burner hearth that installs graphite and catalyst composite material granular sample, feed argon gas; In order to get rid of the air in the microwave burner hearth; In heating roasting reduction process, feeding volume is the mixed gas of 2% hydrogen and 98% argon gas, and the total feeding amount of mixed gas and the relation of graphite and catalyst composite material granular are 0.75m
3/ kg rapid heating is warming up to 1050 ℃, and 1050 ℃ of insulation 50min under the mixed gas of 2% hydrogen and 98% argon gas are cooled to 40 ℃ with bottom discharge again, and then that roasting reduction is good catalyst composite material granular packs.
Embodiment 3:
At first in the microwave burner hearth that installs graphite and catalyst composite material granular sample, feed nitrogen; In order to get rid of the air in the microwave burner hearth; In heating roasting reduction process, feeding volume is the mixed gas of 6% hydrogen and 94% nitrogen, and the total feeding amount of mixed gas and the relation of graphite and catalyst composite material granular are 0.60m
3/ kg rapid heating is warming up to 1080 ℃, and 1080 ℃ of insulation 40min under the mixed gas of 6% hydrogen and 94% nitrogen are cooled to 50 ℃ with bottom discharge again, and then that roasting reduction is good catalyst composite material granular packs.
Embodiment 4:
At first in the microwave burner hearth that installs graphite and catalyst composite material granular sample, feed argon gas; In order to get rid of the air in the microwave burner hearth; In heating roasting reduction process, feeding volume is the mixed gas of 10% hydrogen and 90% argon gas, and the total feeding amount of mixed gas and the relation of graphite and catalyst composite material granular are 0.50m
3/ kg rapid heating is warming up to 1100 ℃, and 1100 ℃ of insulation 30min under the mixed gas of 10% hydrogen and 90% argon gas are cooled to 60 ℃ with bottom discharge again, and then that roasting reduction is good catalyst composite material granular packs.
Claims (3)
1. the method for reducing of graphite for diamond synthesis and catalyst composite material granular; It is characterized in that: comprise following process step: graphite and catalyst composite material granular are put into microwave kiln; Elder generation feeds rare gas element and gets rid of the air in the microwave kiln, and feeding and rare gas element volume ratio are 2%～10% H again
2, at rare gas element and H
2Mixed atmosphere in utilize microwave heating to be rapidly heated to 1050～1100 ℃, at top temperature place insulation 30～60min, be cooled to 60 ℃ at last then with bottom discharge, pack immediately after the discharging.
2. the method for reducing of graphite for diamond synthesis according to claim 1 and catalyst composite material granular is characterized in that: said rare gas element is nitrogen or argon gas.
3. the method for reducing of graphite for diamond synthesis according to claim 1 and 2 and catalyst composite material granular is characterized in that: the total feeding amount of described mixed gas and the relation of graphite and catalyst composite material granular are 0.50～0.75m
3/ kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104289553A CN102557024A (en) | 2011-12-20 | 2011-12-20 | Reduction method of composite material particles of graphite for synthetic diamond and contact agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104289553A CN102557024A (en) | 2011-12-20 | 2011-12-20 | Reduction method of composite material particles of graphite for synthetic diamond and contact agent |
Publications (1)
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|---|---|
| CN102557024A true CN102557024A (en) | 2012-07-11 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN2011104289553A Pending CN102557024A (en) | 2011-12-20 | 2011-12-20 | Reduction method of composite material particles of graphite for synthetic diamond and contact agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111437773A (en) * | 2020-04-21 | 2020-07-24 | 江苏卓远半导体有限公司 | Process for crystallizing diamond single crystal at high temperature by microwave gas |
| CN116813348A (en) * | 2023-07-11 | 2023-09-29 | 聊城冠县尚敖超硬材料有限公司 | Reduction treatment method and process for high-yield graphite column |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2102316C1 (en) * | 1990-04-27 | 1998-01-20 | Олег Александрович Гололобов | Method of preparing batch for diamond synthesis |
| CN101628715A (en) * | 2008-07-14 | 2010-01-20 | 湖北鄂信钻石材料有限责任公司 | Method for preparing powder material special for type I synthetic diamond |
| CN101837267A (en) * | 2010-06-02 | 2010-09-22 | 山东聊城昌润超硬材料有限公司 | Prismatic crystal diamond synthesizing process |
| CN102233251A (en) * | 2011-07-08 | 2011-11-09 | 河南金渠黄金股份有限公司 | Abrasive-level diamond nucleating agent |
-
2011
- 2011-12-20 CN CN2011104289553A patent/CN102557024A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2102316C1 (en) * | 1990-04-27 | 1998-01-20 | Олег Александрович Гололобов | Method of preparing batch for diamond synthesis |
| CN101628715A (en) * | 2008-07-14 | 2010-01-20 | 湖北鄂信钻石材料有限责任公司 | Method for preparing powder material special for type I synthetic diamond |
| CN101837267A (en) * | 2010-06-02 | 2010-09-22 | 山东聊城昌润超硬材料有限公司 | Prismatic crystal diamond synthesizing process |
| CN102233251A (en) * | 2011-07-08 | 2011-11-09 | 河南金渠黄金股份有限公司 | Abrasive-level diamond nucleating agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111437773A (en) * | 2020-04-21 | 2020-07-24 | 江苏卓远半导体有限公司 | Process for crystallizing diamond single crystal at high temperature by microwave gas |
| CN116813348A (en) * | 2023-07-11 | 2023-09-29 | 聊城冠县尚敖超硬材料有限公司 | Reduction treatment method and process for high-yield graphite column |
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Application publication date: 20120711 |