CN113618057A - Powder metallurgy method for preparing sheet catalyst for synthesizing large single crystal diamond - Google Patents

Powder metallurgy method for preparing sheet catalyst for synthesizing large single crystal diamond Download PDF

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Publication number
CN113618057A
CN113618057A CN202010377253.6A CN202010377253A CN113618057A CN 113618057 A CN113618057 A CN 113618057A CN 202010377253 A CN202010377253 A CN 202010377253A CN 113618057 A CN113618057 A CN 113618057A
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China
Prior art keywords
single crystal
catalyst
crystal diamond
large single
metal powder
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CN202010377253.6A
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Chinese (zh)
Inventor
吴旭阳
胡军恒
李建华
董大伟
张恒涛
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Henan Huanghe Whirlwind Co Ltd
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Henan Huanghe Whirlwind Co Ltd
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Priority to CN202010377253.6A priority Critical patent/CN113618057A/en
Publication of CN113618057A publication Critical patent/CN113618057A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85Chromium, molybdenum or tungsten
    • B01J23/86Chromium
    • B01J23/868Chromium copper and chromium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • B22F3/03Press-moulding apparatus therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/06Ferrous alloys, e.g. steel alloys containing aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/42Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C38/00Ferrous alloys, e.g. steel alloys
    • C22C38/18Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/40Ferrous alloys, e.g. steel alloys containing chromium with nickel
    • C22C38/52Ferrous alloys, e.g. steel alloys containing chromium with nickel with cobalt

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Catalysts (AREA)

Abstract

The invention discloses a flaky catalyst for synthesizing large single crystal diamond prepared by a powder metallurgy method, which comprises the following steps: (1) weighing a certain amount of metal powder as required; (2) putting the weighed metal powder into mixing equipment for mixing; (3) putting the uniformly mixed metal powder into a die to be pressed into a required shape; (4) the pressed blank with the die is put into a vacuum sintering furnace for sintering to form the catalyst which can be directly used.

Description

Powder metallurgy method for preparing sheet catalyst for synthesizing large single crystal diamond
Technical Field
The invention belongs to the technical field of processing technology of a sheet catalyst for synthesizing large single crystal diamond, and particularly relates to a powder metallurgy method for preparing the sheet catalyst for synthesizing the large single crystal diamond.
Background
The traditional preparation process of the sheet catalyst comprises the steps of smelting iron-nickel-cobalt with a proper proportion, casting the smelted iron-nickel-cobalt into a round nail or a square ingot, then cold rolling and cutting the round nail or the square ingot to prepare the sheet catalyst into a required shape (generally a wafer), wherein in the processes of high-temperature smelting, casting, later cold rolling and cutting, the catalyst alloy is easily polluted by external materials, so that the catalyst performance is unstable, meanwhile, the material loss is serious in the processes of smelting, casting and cutting, the utilization rate is low, at present, part of laboratories adopt a surface coating method to prepare the catalyst alloy, but the production cost is high, the catalyst components are uneven and difficult to put into production, and aiming at the problem, the invention designs the sheet catalyst for synthesizing the large single crystal diamond by using an end-metallurgy method.
Disclosure of Invention
In order to solve the problems, the invention mainly aims to design a powder metallurgy method for preparing a sheet catalyst for synthesizing large single crystal diamond, metal powder is directly mixed according to a certain proportion and then prepared into a required shape by the powder metallurgy method, the material utilization rate is high, the pollution degree in the processing process is low, the catalyst performance is stable, and the comprehensive benefit is high.
In order to achieve the purpose, the invention adopts the following technical scheme:
a powder metallurgy method for preparing a sheet catalyst for synthesizing large single crystal diamond comprises the following steps:
(1) weighing a certain amount of metal powder as required;
(2) putting the weighed metal powder into mixing equipment for mixing;
(3) putting the uniformly mixed metal powder into a die to be pressed into a required shape;
(4) putting the pressed blank together with the die into a vacuum sintering furnace for sintering;
(5) the catalyst is formed after sintering, and can be directly used.
As a further description of the present invention, the metal powder uniformly mixed in step (3) may also be directly placed in a mold without pressing, and in step (4), the mold containing the metal powder is placed in a vacuum sintering furnace for sintering.
As a further description of the invention, the metal powder in step (1) comprises three elements, wherein the first element is iron, the second element is nickel and cobalt, and the third element is chromium, aluminum and copper.
As a further description of the invention, the weight ratios of the three elements in the step (1) are respectively as follows:
iron: 50-80%, nickel and cobalt in total: 45-15%, chromium, aluminum and copper in total: 0.1 to 5 percent.
As a further description of the invention, in the step (2), the material of the inner wall of the mixing device is stainless steel or high-density ceramic.
As a further description of the invention, in the step (3), the die is made of die steel or high-density ceramic or high-purity graphite.
As a further description of the invention, in the step (4), the sintering temperature of the vacuum sintering furnace is 750-1300 ℃, and the vacuum degree in the sintering process is not lower than 1 x 10-1Pa。
Compared with the prior art, the invention has the technical effects that:
the invention provides a flaky catalyst for synthesizing large single crystal diamond prepared by a powder metallurgy method, the catalyst alloy preparation process adopted by the invention has the advantages of low metal powder loss, utilization rate of more than 90 percent and low cost, and the traditional smelting-casting-cutting process is difficult to reach 50 percent;
in the processing process of the catalyst alloy, the controllability of the materials of mixing equipment and a die is good, the pollution degree of the catalyst is obviously reduced, the components are stable, and the catalyst is seriously polluted and the components are difficult to keep stable due to the existence of a crucible, a pouring gate and cutting fluid in the traditional process;
the preparation process of the powder metallurgy method has the advantages of convenient component adjustment, capability of adjusting the components of the catalyst at any time, short component adjustment period and low cost, and the traditional process for adjusting the catalyst needs to replace a crucible and a sprue again, so the period is long and the cost is high.
Detailed Description
The present invention is described in detail below:
a powder metallurgy method for preparing a sheet catalyst for synthesizing large single crystal diamond comprises the following steps:
(1) weighing a certain amount of metal powder as required;
(2) putting the weighed metal powder into mixing equipment for mixing;
(3) putting the uniformly mixed metal powder into a die to be pressed into a required shape;
(4) putting the pressed blank together with the die into a vacuum sintering furnace for sintering;
(5) the catalyst is formed after sintering, and can be directly used.
And (4) putting the mould containing the metal powder into a vacuum sintering furnace for sintering.
The metal powder in the step (1) comprises three elements, wherein the first element is iron, the second element is nickel and cobalt, and the third element is chromium, aluminum and copper.
The weight ratios of the three elements in the step (1) are respectively as follows:
iron: 50-80%, nickel and cobalt in total: 45-15%, chromium, aluminum and copper in total: 0.1 to 5 percent.
The metal powder comprises but is not limited to iron, nickel and cobalt elementary powder or pre-alloy powder, and elements such as zirconium, aluminum, titanium, sulfur, phosphorus, boron and the like are added according to the performance requirement of the large single crystal diamond.
The granularity of each powder is-50 to-1000 meshes.
The inner wall of the mixing device in the step (2) is made of stainless steel or high-density ceramic, and the influence on catalyst components in the mixing process is small.
The material of the die in the step (3) is die steel, high-density ceramic or high-purity graphite.
The die material includes but not limited to die steel, hard alloy, ceramic, high-purity graphite, the material is difficult to get into the alloy powder in the course of pressing and sintering, do not react with catalyst alloy powder, will not cause the pollution to the catalyst.
The sintering process of the vacuum sintering furnace in the step (4) adopts a common powder metallurgy sintering process, the sintering temperature is 750-1300 ℃, and the vacuum degree in the sintering process is not lower than 1 x 10-1Pa。
The invention is divided into the following embodiments according to the difference of metal powder and sintering conditions, and the specific implementation mode is as follows:
example 1:
the powder metallurgy method for preparing the flaky catalyst for synthesizing the large single crystal diamond comprises the following steps:
(1) weighing metal powder according to the following weight ratio: 50% of first element, 49.9% of second element and 0.1% of third element;
(2) putting the weighed metal powder into mixing equipment for mixing;
(3) putting the uniformly mixed metal powder into a mould to be pressed into a required shape or directly putting the metal powder into the mould;
(4) the pressed green body is put into a vacuum sintering furnace together with a mold or directly put into a mold containing metal powder for sintering, the sintering temperature is 750 ℃, and the vacuum degree is 2 x 10 in the sintering process-1Pa。
Example 2:
the powder metallurgy method for preparing the flaky catalyst for synthesizing the large single crystal diamond comprises the following steps:
(1) weighing metal powder according to the following weight ratio: 80% of first element, 15% of second element and 5% of third element;
(2) putting the weighed metal powder into mixing equipment for mixing;
(3) putting the uniformly mixed metal powder into a mould to be pressed into a required shape or directly putting the metal powder into the mould;
(4) the pressed green body is put into a vacuum sintering furnace together with a mold or directly put into a mold containing metal powder for sintering, the sintering temperature is 1300 ℃, and the vacuum degree is 5 x 10 in the sintering process-1Pa。
Example 3:
the powder metallurgy method for preparing the flaky catalyst for synthesizing the large single crystal diamond comprises the following steps:
(1) weighing metal powder according to the following weight ratio: 70% of first element, 27% of second element and 3% of third element;
(2) putting the weighed metal powder into mixing equipment for mixing;
(3) putting the uniformly mixed metal powder into a mould to be pressed into a required shape or directly putting the metal powder into the mould;
(4) the pressed green body is put into a vacuum sintering furnace together with a mold or directly put into a mold containing metal powder for sintering, the sintering temperature is 1000 ℃, and the vacuum degree is 3 x 10 in the sintering process-1Pa。
The invention provides a flaky catalyst for synthesizing large single crystal diamond prepared by a powder metallurgy method, the catalyst alloy preparation process adopted by the invention has the advantages of low metal powder loss, utilization rate of more than 90 percent and low cost, and the traditional smelting-casting-cutting process is difficult to reach 50 percent;
in the processing process of the catalyst alloy, the controllability of the materials of mixing equipment and a die is good, the pollution degree of the catalyst is obviously reduced, the components are stable, and the catalyst is seriously polluted and the components are difficult to keep stable due to the existence of a crucible, a pouring gate and cutting fluid in the traditional process;
the preparation process of the powder metallurgy method has the advantages of convenient component adjustment, capability of adjusting the components of the catalyst at any time, short component adjustment period and low cost, and the traditional process for adjusting the catalyst needs to replace a crucible and a sprue again, so the period is long and the cost is high.
The real density of the catalyst alloy prepared by the powder metallurgy method reaches more than 80 percent of the theoretical density.
The above embodiments are only for illustrating the technical solutions of the present invention and are not limited, and other modifications or equivalent substitutions made by the technical solutions of the present invention by the ordinary skilled person in the art are included in the scope of the claims of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (7)

1. A powder metallurgy method for preparing a sheet catalyst for synthesizing large single crystal diamond is characterized in that: the method comprises the following steps:
(1) weighing a certain amount of metal powder as required;
(2) putting the weighed metal powder into mixing equipment for mixing;
(3) putting the uniformly mixed metal powder into a die to be pressed into a required shape;
(4) putting the pressed blank together with the die into a vacuum sintering furnace for sintering;
(5) the catalyst is formed after sintering, and can be directly used.
2. The powder metallurgy method for preparing a sheet catalyst for synthesizing large single crystal diamond according to claim 1, wherein: and (4) putting the mould containing the metal powder into a vacuum sintering furnace for sintering.
3. The powder metallurgy method for preparing a sheet catalyst for large single crystal diamond synthesis according to claim 1 or 2, wherein: the metal powder in the step (1) comprises three elements, wherein the first element is iron, the second element is nickel and cobalt, and the third element is chromium, aluminum and copper.
4. The powder metallurgy method for preparing sheet catalyst for synthesizing large single crystal diamond according to claim 3, wherein: the weight ratios of the three elements in the step (1) are respectively as follows:
iron: 50-80%, nickel and cobalt in total: 45-15%, chromium, aluminum and copper in total: 0.1 to 5 percent.
5. The powder metallurgy method for preparing a sheet catalyst for synthesizing large single crystal diamond according to claim 1, wherein: the inner wall of the mixing equipment in the step (2) is made of stainless steel or high-density ceramic.
6. The powder metallurgy method for preparing a sheet catalyst for large single crystal diamond synthesis according to claim 1 or 2, wherein: and (4) adopting die steel or high-density ceramic or high-purity graphite as the die in the step (3).
7. The powder metallurgy method for preparing a sheet catalyst for large single crystal diamond synthesis according to claim 1 or 2, wherein: the sintering temperature of the vacuum sintering furnace in the step (4) is 750-1300 ℃, and the vacuum degree in the sintering process is not lower than 1 x 10-1Pa。
CN202010377253.6A 2020-05-07 2020-05-07 Powder metallurgy method for preparing sheet catalyst for synthesizing large single crystal diamond Pending CN113618057A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1105903A (en) * 1994-01-24 1995-08-02 成都科技大学 Method of synthetizing diamond with silicon carbide and metal
WO2004067211A1 (en) * 2003-01-31 2004-08-12 Toho Titanium Co., Ltd. Fine metal powder, process for producing the same, and conductive paste containing the fine metal powder
CN101024155A (en) * 2007-01-16 2007-08-29 山东建筑大学 Powdered metallurgy catalyst for synthesizing high-strength diamond
CN107470625A (en) * 2017-08-15 2017-12-15 唐山国丰钢铁有限公司 A kind of powder metallurgy process for preparing high-purity material
CN109225238A (en) * 2018-08-31 2019-01-18 中南钻石有限公司 A kind of Gem Grade colorless diamond catalyst and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1105903A (en) * 1994-01-24 1995-08-02 成都科技大学 Method of synthetizing diamond with silicon carbide and metal
WO2004067211A1 (en) * 2003-01-31 2004-08-12 Toho Titanium Co., Ltd. Fine metal powder, process for producing the same, and conductive paste containing the fine metal powder
CN101024155A (en) * 2007-01-16 2007-08-29 山东建筑大学 Powdered metallurgy catalyst for synthesizing high-strength diamond
CN107470625A (en) * 2017-08-15 2017-12-15 唐山国丰钢铁有限公司 A kind of powder metallurgy process for preparing high-purity material
CN109225238A (en) * 2018-08-31 2019-01-18 中南钻石有限公司 A kind of Gem Grade colorless diamond catalyst and preparation method thereof

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