CN100425333C - Method for preparing cementite - Google Patents

Method for preparing cementite Download PDF

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Publication number
CN100425333C
CN100425333C CNB2007100130679A CN200710013067A CN100425333C CN 100425333 C CN100425333 C CN 100425333C CN B2007100130679 A CNB2007100130679 A CN B2007100130679A CN 200710013067 A CN200710013067 A CN 200710013067A CN 100425333 C CN100425333 C CN 100425333C
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China
Prior art keywords
cementite
weight
pyrophillite
powder
diamond
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Expired - Fee Related
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CNB2007100130679A
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Chinese (zh)
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CN101053806A (en
Inventor
崔建军
崔潇
李木森
万桂怡
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Shandong University
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Shandong University
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Abstract

The invention relates to a method for preparing cementite, which has the following steps: A. 80-95 by weight of iron dust, 1-3 by weight of nickel powder, and 3-9 by weight of graphite powder are uniformly mixed, and then is dried; B. the mixing powder is cold press moulding at the pressure of 600-700MPa; C. the surface is clear to get rid of dust; D. 2-5:1 by weight of cold press moulding blank and graphite flake are alternately put into the cavity of pyrophillite which is fixed on the hexahedral anvil presser; and E. the pyrophillite keeps for 90s-4min under the ultra high pressure of 2-5GPa, at the temperature of 1200-1500 degree C. Iron dust, nickel powder graphite powder of a certain proportion react in a certain condition to produce a great lot of cementite, which greatly increases the mass and quantity of man-made diamond. And the cementite prepared by this method has a high output, and improves the continuous formation and growth of the diamond grain in the process of diamond synthesize.

Description

A kind of method for preparing cementite
Technical field
The present invention relates to a kind of preparation method of metal material, specifically a kind of method for preparing cementite.
Background technology
We know that graphitic carbon and diamond are respectively the different expression forms of carbon, belong to the isomer of carbon.Artificially synthesizing diamond, its essence is exactly under manual intervention, the graphite of carbon is constructed be transformed into the diamond structure.669 pages of 2002 " Science Bulletin " the 47th the 9th phases of volume have delivered people such as Xu Bin and have been entitled as " growth of the structure of metal coating and Fe base catalyst diamond synthesis " achievement in research, found transformational relation between graphitic carbon, cementite and the diamond from microstructure in the literary composition, proved by graphitic carbon to be transformed into the process that rearranges that diamond is not a simple carbon atom, but needed through a series of intermediate link.Wherein, the γ of cementite in catalyst-(Fe, under attraction Ni), with carbon atom group with the intermediate structure of sheet form from Fe 3Precipitation among the C, last, this carbon atom group is stacked on the diamond plane surface.Obviously, as the raw material of diamond synthesis, cementite is compared with graphite, and cementite is more near the adamantine raw material of final products.For a long time, extensively adopt catalyst metal to add graphite and become diamond both at home and abroad, in this process, though also can produce cementite, but along with growth of diamond, to produce a large amount of consumption to cementite, owing to due to physics, chemistry and the metallurgy environment in the reaction melt, be can not get replenishing by the used up cementite of growth of diamond, therefore, adamantine continuation forms and grows for want of cementite and stagnate, so the diamond grade of produced in conventional processes is low, granularity is little.
Summary of the invention
The present invention is for overcoming above-mentioned the deficiencies in the prior art, provides that a kind of production technology is simple, cost is low, can produce the preparation method of cementite in a large number.
The objective of the invention is to adopt following technical proposals to realize: a kind of method for preparing cementite, A. mixes 88-95 part iron powder, 1-3 part nickel powder, 3-9 part graphite powder by weight, and moisture is removed in oven dry;
B. with mixed powder cold moudling under 600-700MPa pressure;
C. removing surface, remove crude removal;
D. by weight than being that 2~5: 1 cold moudling stock and graphite flake are alternately put into the pyrophillite cavity and pyrophillite is placed on the cubic hinge press;
E. pyrophillite is imposed the super-pressure, 1200-1350 degree centigrade of 2-5GPa and kept 90 seconds to 4 minutes.
Be sheet or cylindric with mixed powder cold moudling under 600-700MPa pressure among the step B.
The present invention adopts a certain proportion of iron powder, nickel powder and graphite powder is reacted under certain condition, can produce a large amount of cementites, the quality and the quantity of artificially synthesizing diamond will be improved greatly, also the base substance basis of furtheing investigate adamantine formation mechanism and providing research institute to need can be simultaneously the control device that diamond forms.The cementite that utilizes this method to produce, the output height can promote the continuation of diamond particles to form and growth in the diamond building-up process.
Description of drawings
Accompanying drawing is the cementite ESEM picture that embodiment 3 produces.
The specific embodiment
The present invention is further described below in conjunction with drawings and Examples.
Embodiment 1:A. mixes 88 parts of iron powders, 1 part of nickel powder, 3 parts of graphite powders by weight, and moisture is removed in oven dry;
B. be sheet with mixed powder cold moudling under 600MPa pressure;
C. removing surface, remove crude removal;
D. by weight than being 2: 1 cold moudling stock and graphite flake are alternately put into the pyrophillite cavity and pyrophillite is placed on the cubic hinge press;
E. pyrophillite is imposed the super-pressure, 1350 degrees centigrade of 5GPa and kept 90 seconds.
Embodiment 2:A. mixes 91 parts of iron powders, 2 parts of nickel powders, 6 parts of graphite powders by weight, and moisture is removed in oven dry;
B. be cylindric with mixed powder cold moudling under 650MPa pressure;
C. removing surface, remove crude removal;
D. by weight than being that 3: 1 cold moudling stock and graphite flake are alternately put into the pyrophillite cavity and pyrophillite is placed on the cubic hinge press;
E. pyrophillite is imposed the super-pressure, 1300 degrees centigrade of 2GPa and kept 2 minutes.
Embodiment 3:A. mixes 95 parts of iron powders, 3 parts of nickel powders, 9 parts of graphite powders by weight, and moisture is removed in oven dry;
B. be cylindric with mixed powder cold moudling under 700MPa pressure;
C. removing surface, remove crude removal;
D. by weight than being that 4: 1 cold moudling stock and graphite flake are alternately put into the pyrophillite cavity and pyrophillite is placed on the cubic hinge press;
E. pyrophillite is imposed the super-pressure, 1200 degrees centigrade of 3GPa and kept 4 minutes.
The cementite that is produced as shown in drawings, therefrom the ratio of cementite reaches more than 90% as can be seen.
Embodiment 4:A. mixes 88 parts of iron powders, 3 parts of nickel powders, 5 parts of graphite powders by weight, and moisture is removed in oven dry;
B. be cylindric with mixed powder cold moudling under 680MPa pressure;
C. removing surface, remove crude removal;
D. by weight than being that 4.5: 1 cold moudling stock and graphite flake are alternately put into the pyrophillite cavity and pyrophillite is placed on the cubic hinge press;
E. pyrophillite is imposed the super-pressure, 1280 degrees centigrade of 4GPa and kept 3 minutes.
Embodiment 5 A. mix 95 parts of iron powders, 1 part of nickel powder, 4 parts of graphite powders by weight, and moisture is removed in oven dry;
B. be sheet with mixed powder cold moudling under 630MPa pressure;
C. removing surface, remove crude removal;
D. by weight than being that 5: 1 cold moudling stock and graphite flake are alternately put into the pyrophillite cavity and pyrophillite is placed on the cubic hinge press;
E. pyrophillite is imposed the super-pressure, 1300 degrees centigrade of 3.5GPa and kept 2 minutes.

Claims (2)

1. method for preparing cementite, it is characterized in that: A. mixes 88-95 part iron powder, 1-3 part nickel powder, 3-9 part graphite powder by weight, and moisture is removed in oven dry;
B. with mixed powder cold moudling under 600-700MPa pressure;
C. removing surface, remove crude removal;
D. by weight than being that 2~5: 1 cold moudling stock and graphite flake are alternately put into the pyrophillite cavity and pyrophillite is placed on the cubic hinge press;
E. pyrophillite is imposed the super-pressure, 1200-1350 degree centigrade of 2-5GPa and kept 90 seconds to 4 minutes.
2. a kind of method for preparing cementite according to claim 1 is characterized in that: be sheet or cylindric with mixed powder cold moudling under 600-700MPa pressure among the step B.
CNB2007100130679A 2007-01-22 2007-01-22 Method for preparing cementite Expired - Fee Related CN100425333C (en)

Priority Applications (1)

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Application Number Priority Date Filing Date Title
CNB2007100130679A CN100425333C (en) 2007-01-22 2007-01-22 Method for preparing cementite

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CN101053806A CN101053806A (en) 2007-10-17
CN100425333C true CN100425333C (en) 2008-10-15

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101628715B (en) * 2008-07-14 2012-08-08 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
CN102784917A (en) * 2011-05-18 2012-11-21 中国石油化工集团公司 Manufacture method for directly combining diamond grind block
CN104313448B (en) * 2014-10-23 2016-08-03 东南大学 Block high-purity cementite of a kind of high-compactness and preparation method thereof
CN115007067B (en) * 2022-06-14 2023-04-25 上海征世科技股份有限公司 Device and method for preparing high-purity monocrystalline diamond piece

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4273561A (en) * 1975-08-27 1981-06-16 Fernandez Moran Villalobos Hum Ultrasharp polycrystalline diamond edges, points, and improved diamond composites, and methods of making and irradiating same
RU1820890C (en) * 1990-11-29 1993-06-07 Институт Высоких Температур Российской Академии Наук Method of artificial diamond making
JPH05168901A (en) * 1991-12-17 1993-07-02 Tatsuro Kuratomi Synthesis of diamond
CN1261553A (en) * 2000-01-31 2000-08-02 山东工业大学 Iron-base alloy catalyst and its preparing method
CN1298757A (en) * 2000-06-30 2001-06-13 朱贵增 Process for preparing microcrystalline diamond

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4273561A (en) * 1975-08-27 1981-06-16 Fernandez Moran Villalobos Hum Ultrasharp polycrystalline diamond edges, points, and improved diamond composites, and methods of making and irradiating same
RU1820890C (en) * 1990-11-29 1993-06-07 Институт Высоких Температур Российской Академии Наук Method of artificial diamond making
JPH05168901A (en) * 1991-12-17 1993-07-02 Tatsuro Kuratomi Synthesis of diamond
CN1261553A (en) * 2000-01-31 2000-08-02 山东工业大学 Iron-base alloy catalyst and its preparing method
CN1298757A (en) * 2000-06-30 2001-06-13 朱贵增 Process for preparing microcrystalline diamond

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
渗碳体高温高压金刚石化的显微分析. 李洪岩等.金刚石与磨料磨具工程,第152卷第2期. 2006
渗碳体高温高压金刚石化的显微分析. 李洪岩等.金刚石与磨料磨具工程,第152卷第2期. 2006 *
铁基触媒中的初生渗碳体与金刚石单晶的合成. 崔建军等.金刚石与磨料磨具工程,第146卷第2期. 2005
铁基触媒中的初生渗碳体与金刚石单晶的合成. 崔建军等.金刚石与磨料磨具工程,第146卷第2期. 2005 *

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Assignee: Hubei E-Xin Diamond Material Co., Ltd.

Assignor: Shandong University

Contract record no.: 2011420000088

Denomination of invention: Method for preparing cementite

Granted publication date: 20081015

License type: Exclusive License

Open date: 20071017

Record date: 20110517

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CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20081015

Termination date: 20130122