CN117245094A - Method for filling and synthesizing thick-layer superhard material composite sheet - Google Patents

Method for filling and synthesizing thick-layer superhard material composite sheet Download PDF

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Publication number
CN117245094A
CN117245094A CN202311244177.1A CN202311244177A CN117245094A CN 117245094 A CN117245094 A CN 117245094A CN 202311244177 A CN202311244177 A CN 202311244177A CN 117245094 A CN117245094 A CN 117245094A
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China
Prior art keywords
composite sheet
powder
superhard material
thick
material composite
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Application number
CN202311244177.1A
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Chinese (zh)
Inventor
陈家荣
胡乔帆
陈超
莫培程
潘晓毅
张俊
李凯
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China Nonferrous Metal Guilin Geology and Mining Co Ltd
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China Nonferrous Metal Guilin Geology and Mining Co Ltd
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Priority to CN202311244177.1A priority Critical patent/CN117245094A/en
Publication of CN117245094A publication Critical patent/CN117245094A/en
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    • 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
    • B22F7/00Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/02Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
    • 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

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a filling synthesis method of a thick-layer superhard material composite sheet, which relates to the technical field of superhard material composite sheet synthesis and comprises the following steps: (1) Uniformly mixing the superhard powder and the powder serving as a catalyst and a binder to obtain mixed powder; (2) Flatly laying the mixed powder into a metal cup, covering a hard alloy matrix on the surface of the mixed powder, and covering the metal cup to obtain a preassembled composite sheet; (3) Wrapping the pre-assembled composite sheet by a metal foil, wrapping by a pressure-transmitting powder, and then placing in a compacting die for compacting; (4) Demolding, taking out the preassembled composite sheet, and purifying and shaping at high temperature in a vacuum environment to obtain a purified and shaped composite sheet; (5) And (3) placing the purified and shaped composite sheet in a heat-preserving pressure-transmitting medium, and synthesizing at high temperature and high pressure to obtain the thick-layer superhard material composite sheet. The invention ensures that the metal cup is uniformly contracted when compacting powder, can realize the synthesis of thick-layer superhard material composite sheets and prolongs the service life of the compacting die.

Description

Method for filling and synthesizing thick-layer superhard material composite sheet
Technical Field
The invention relates to the technical field of superhard material composite sheet synthesis, in particular to a filling synthesis method of a thick-layer superhard material composite sheet.
Background
The diamond or cubic boron nitride composite sheet belongs to a superhard material composite sheet, and is a superhard material polymerized on the surface of a hard alloy substrate by taking diamond or cubic boron nitride particles as main materials. The super-hard material composite sheet has the characteristics of high hardness and good wear resistance, is widely applied to industries such as petroleum drilling, geological exploration, coal field drilling and production drill bit, machining tools and the like, and is widely applied to tool machining. In particular to cutting machining in machining, superhard material composite sheets are applied to the cutter industry, and along with the continuous development of the machining industry, the application range is wider and wider, wherein the superhard material composite sheets comprise a common lathe tool, a common machining drill bit, a common milling cutter for frame machining and a common copying milling cutter. The precision requirement of a workpiece is higher and higher under the influence of processing requirements, the requirement on a superhard material cutter is higher and higher, the thickness of a polycrystalline layer of a superhard material composite sheet is only 0.5-1.2mm under the common condition, but the application advantage of the superhard material composite sheet with large thickness in a milling cutter is more outstanding, the superhard material composite sheet is more suitable for the production of the milling cutter with a rotating surface, the influence of high difficulty in the synthesis of the superhard material composite sheet with large thickness is more suitable for the production of the milling cutter with a rotating surface, and the synthesis of diamond or cubic boron nitride composite sheet with large thickness is difficult to obtain a consistent product, so that many enterprises are unwilling to develop, particularly the synthesis of the superhard material composite sheet with large thickness with the granularity of less than 10 microns is more difficult, the non-sintering phenomenon is easy to occur at the center of the polycrystalline layer, and the influence of uneven compaction of powder in the earlier stage is mainly affected. The diamond or cubic boron nitride powder is filled into rare metal thin cups with the thickness of only 0.5-0.22mm, when a large amount of powder is filled into the rare metal thin cups, the expansion diameter of the metal thin cups is enlarged by compacting the powder, the outer diameter of the metal thin cups cannot be kept in the original shape, the core is difficult to sinter or crack due to inconsistent edge shrinkage and core shrinkage in the synthesis process, meanwhile, tantalum cups, niobium cups, zirconium cups or molybdenum cups used in the composite sheet synthesis process are of relatively soft metal materials and are easy to mold, when the size of a die made of die steel is controlled, the metal thin cups are easy to deform into die gaps, and the die life is very short due to abrasion of the residual superhard material cubic boron nitride powder and diamond powder on the die walls in a die clamping mode.
Disclosure of Invention
The invention aims to provide a filling synthesis method of a thick-layer superhard material composite sheet, which solves the problems in the prior art, ensures that a metal cup is uniformly contracted when powder is compacted, can realize the synthesis of the thick-layer superhard material composite sheet, and prolongs the service life of a compacting die.
In order to achieve the above object, the present invention provides the following solutions:
the invention provides a loading synthesis method of a thick-layer superhard material composite sheet, which comprises the following steps:
(1) Uniformly mixing the superhard powder and the powder serving as a catalyst and a binder to obtain mixed powder;
(2) Flatly laying the mixed powder into a metal cup, covering a hard alloy matrix on the surface of the mixed powder, and covering the metal cup to obtain a preassembled composite sheet;
(3) Wrapping the preassembled composite sheet by a metal foil, wrapping by a pressure-transmitting powder, and then placing in a compacting die for compacting;
(4) Demolding, taking out the preassembled composite sheet, and purifying and shaping at high temperature in a vacuum environment to obtain a purified and shaped composite sheet;
(5) And placing the purification and shaping composite sheet in a heat-preserving pressure-transmitting medium for high-temperature and high-pressure synthesis to obtain the thick-layer superhard material composite sheet.
Preferably, the superhard powder is one or both of diamond and cubic boron nitride.
Preferably, the powder as the catalyst and the binder is one or both of cobalt powder and tantalum powder.
Preferably, the metal cup is a tantalum cup, a niobium cup, a zirconium cup or a molybdenum cup, and the cup cover of the metal cup is a tantalum cover, a niobium cover, a zirconium cover or a molybdenum cover.
Preferably, in step (3), the compaction is performed in the compaction tool at a pressure of 3 to 5 tons.
Preferably, in step (4), at 10 -2 ~10 -5 And (3) carrying out high-temperature purification and shaping at 600-1100 ℃ in Pa vacuum environment for 1-3 hours.
Preferably, in the step (5), the conditions of high temperature and high pressure synthesis are: the pressure is 5.5-7.5GPa, the temperature is 1500-1800 ℃, and the heat preservation time is 10-20min.
Preferably, in step (3), the pre-assembled composite sheets wrapped by at least one metal foil are put into a compacting die, and the metal foil outside each pre-assembled composite sheet is wrapped by pressure-transmitting powder material, and each pre-assembled composite sheet is compacted.
Compared with the prior art, the invention has the following technical effects:
the invention provides a filling synthesis method of a thick-layer superhard material composite sheet, which comprises the steps of wrapping a pre-filled composite sheet by a metal foil, wrapping the pre-filled composite sheet by a pressure-transmitting powder material, and then compacting the pre-filled composite sheet in a compacting die, so that a metal cup is uniformly contracted when compacting powder materials, the metal cup is separated from the compacting die by the pressure-transmitting powder materials and the metal foil, the superhard powder materials are prevented from wearing the wall surface of the compacting die, and the service life of the compacting die is prolonged.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of simultaneous compaction of four pre-assembled compacts in an embodiment of the invention;
in the figure: 1-mixed powder, 2-metal cup, 3-hard alloy matrix, 4-metal foil, 5-pressure transmission powder, 6-compaction die, 61-die sleeve and 62-die pressing head.
Detailed Description
As shown in fig. 1, the invention provides a loading synthesis method of a thick-layer superhard material composite sheet, which comprises the following steps:
(1) Uniformly mixing the superhard powder and the powder serving as a catalyst and a binder to obtain a mixed powder 1;
(2) Flatly laying the mixed powder 1 into a metal cup 2, covering a hard alloy matrix 3 on the surface of the mixed powder 1, and covering the metal cup 2 to obtain a preassembled composite sheet;
(3) Wrapping the pre-assembled composite sheet by using a metal foil 4, wrapping the pre-assembled composite sheet by using a pressure-transmitting powder 5, and then placing the pre-assembled composite sheet in a compacting die 6 for compacting;
(4) Demolding, taking out the preassembled composite sheet, and purifying and shaping at high temperature in a vacuum environment to obtain a purified and shaped composite sheet;
(5) And (3) placing the purified and shaped composite sheet in a heat-preserving pressure-transmitting medium, and synthesizing at high temperature and high pressure to obtain the thick-layer superhard material composite sheet.
As an embodiment of the present invention, the ultra-hard powder is one or both of diamond and cubic boron nitride. The diamond particle size is 2-120 μm, preferably 10 μm, and the cubic boron nitride particle size is 5-30 μm, preferably 10 μm. The grain size of the diamond is 2-120 mu m, the grain size of the cubic boron nitride is 5-30 mu m, and the grain size of the cubic boron nitride is the grain size of the main material. When diamond is used as a main material, cubic boron nitride can be added as an ingredient to play a role in toughening; when the cubic boron nitride is used as a material, the particle size range is selected according to actual requirements.
As an embodiment of the present invention, the powder as the catalyst and the binder is one or both of cobalt powder and tantalum powder. The particle size of the cobalt powder is 0.3-5 μm, preferably 2 μm, and the particle size of the tantalum powder is 0.3-5 μm, preferably 2 μm.
As one embodiment of the invention, the superhard powder and the powder serving as the catalyst and the binder are ball-milled in a stainless steel tank of an organic solvent for 1-5 hours, preferably 3 hours, and then dried and screened to obtain the mixed powder 1. Wherein the drying temperature is 60-120deg.C, preferably 80deg.C, and sieving with 80-150 mesh sieve, preferably 100 mesh sieve.
As an embodiment of the present invention, the cemented carbide substrate 3 covered on the surface of the powder mix 1 has a thickness of 2.5-12mm, preferably 8mm, and the cemented carbide substrate 3 is a tungsten carbide-cobalt alloy such as cemented carbides with the designations YG10 to YG18, preferably YG16.
As an embodiment of the present invention, the pressure-transmitting powder 5 may be wrapped with carbon powder, salt powder or tube which is made of carbon or salt in advance and can be matched with a graphite tube, a salt tube, etc. which are filled with pre-assembled composite sheets and are suitable for uniformly transmitting pressure.
As an embodiment of the present invention, the metal cup 2 is a tantalum cup, a niobium cup, a zirconium cup or a molybdenum cup, preferably a niobium cup, and the lid of the metal cup 2 is a tantalum lid, a niobium lid, a zirconium lid or a molybdenum lid, preferably a molybdenum lid.
As an embodiment of the invention, in step (3), the compaction is performed in the compaction tool 6 at a pressure of 3 to 5 tons, preferably 4 tons.
As an embodiment of the present invention, in step (4), at 10 -2 ~10 -5 Under Pa vacuum, preferably 10 -4 And (3) Pa, high-temperature purification and shaping are carried out at 600-1100 ℃ for 1-3 hours.
As an embodiment of the present invention, in the step (5), the conditions of the high-temperature high-pressure synthesis are: the pressure is 5.5-7.5GPa, the temperature is 1500-1800 ℃, and the heat preservation time is 10-20min.
As one embodiment of the invention, the heat-insulating pressure-transmitting medium is pyrophyllite blocks, the purifying and shaping composite sheet is matched with the proper pyrophyllite blocks, and the thick-layer superhard material composite sheet is synthesized in the high temperature and high pressure of the hexahedral press.
As an example of the invention, the layer thickness of the polycrystalline layer of superhard material in a thick layer superhard material compact may be up to 6mm.
As an embodiment of the present invention, in step (3), at least one pre-assembled composite sheet wrapped by the metal foil 4 is placed in the compacting mold 6, and the metal foil 4 outside each pre-assembled composite sheet is wrapped by the pressure-transmitting powder 5, and at the same time, each pre-assembled composite sheet is compacted, and 1 to 20 pre-assembled composite sheets can be compacted at the same time.
The invention will be described in further detail with reference to the drawings and the detailed description.
Example 1
(1) 88g of diamond micropowder with the granularity of 10 mu m, 6g of cubic boron nitride with the granularity of 2 mu m, 4g of cobalt powder with the granularity of 2 mu m and 2g of tantalum powder with the granularity of 2 mu m are ball-milled for 3 hours in a stainless steel tank with an organic solvent, dried at 80 ℃, and sieved by a 100-mesh sieve to obtain diamond micropowder mixed with a catalyst and a binder; in the embodiment, diamond micro powder is used as a main material, and cubic boron nitride is used as an ingredient;
(2) 15.5g of diamond micropowder mixed with a catalyst and a binder are flatly paved and filled into a niobium cup with the diameter of 35mm and covered with hard alloy (tungsten carbide-cobalt) with the thickness of 8mm, and a molybdenum cover is matched, so that a preassembled composite sheet is obtained;
(3) Wrapping the pre-assembled composite sheet by using titanium foil, then wrapping a layer of graphite powder, filling the wrapped composite sheet into a mold sleeve 61, blocking two ends of the mold sleeve 61 by using a mold pressing head 62, applying pressure of 4 tons at the two ends, maintaining the pressure for 15 seconds, and demolding;
(4) The compacted pre-assembled composite sheet is at 10 -4 Preserving the temperature of 700 ℃ in a Pa vacuum furnace for 2 hours to obtain a purifying and shaping composite sheet;
(5) Matching the purifying and shaping composite sheet with proper pyrophyllite blocks, and synthesizing a thick-layer superhard material composite sheet in the high temperature and high pressure of a hexahedral press under the following conditions: the pressure is 6.5GPa, the temperature is 1700 ℃, and the heat preservation is carried out for 15 minutes; and (5) decompressing to obtain the diamond compact with the thickness of the polycrystalline layer of 4.5 mm.
Example 2
(1) 88g of diamond micropowder with the granularity of 10 mu m, 6g of cubic boron nitride with the granularity of 2 mu m, 4g of cobalt powder with the granularity of 2 mu m and 2g of tantalum powder with the granularity of 2 mu m are ball-milled for 3 hours in a stainless steel tank with an organic solvent, dried at 80 ℃, and sieved by a 100-mesh sieve to obtain diamond micropowder mixed with a catalyst and a binder; in the embodiment, diamond micro powder is used as a main material, and cubic boron nitride is used as an ingredient;
(2) 19g of diamond micro powder mixed with a catalyst and an adhesive is tiled and put into a niobium cup with the diameter of 35mm and covered with hard alloy (tungsten carbide-cobalt) with the thickness of 8mm, and a molybdenum cover is matched, so that a preassembled composite sheet is obtained;
(3) Wrapping the preassembled composite sheet by using tinfoil paper, then wrapping a layer of salt powder, filling the salt powder into a mold sleeve 61, blocking two ends of the mold sleeve 61 by using a mold pressing head 62, applying pressure of 4 tons at the two ends, maintaining the pressure for 15 seconds, and demolding;
(4) The compacted pre-assembled composite sheet is at 10 -4 Preserving the temperature of 700 ℃ in a Pa vacuum furnace for 2 hours to obtain a purifying and shaping composite sheet;
(5) Matching the purifying and shaping composite sheet with proper pyrophyllite blocks, and synthesizing a thick-layer superhard material composite sheet in the high temperature and high pressure of a hexahedral press under the following conditions: the pressure is 6.5GPa, the temperature is 1700 ℃, and the heat preservation is carried out for 15 minutes; and (5) decompressing to obtain the diamond compact with the thickness of the polycrystalline layer of 5.5 mm.
The principles and embodiments of the present invention have been described in detail with reference to specific examples, which are provided to facilitate understanding of the method and core ideas of the present invention; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.

Claims (8)

1. The filling synthesis method of the thick-layer superhard material composite sheet is characterized by comprising the following steps of:
(1) Uniformly mixing the superhard powder and the powder serving as a catalyst and a binder to obtain mixed powder;
(2) Flatly laying the mixed powder into a metal cup, covering a hard alloy matrix on the surface of the mixed powder, and covering the metal cup to obtain a preassembled composite sheet;
(3) Wrapping the preassembled composite sheet by a metal foil, wrapping by a pressure-transmitting powder, and then placing in a compacting die for compacting;
(4) Demolding, taking out the preassembled composite sheet, and purifying and shaping at high temperature in a vacuum environment to obtain a purified and shaped composite sheet;
(5) And placing the purification and shaping composite sheet in a heat-preserving pressure-transmitting medium for high-temperature and high-pressure synthesis to obtain the thick-layer superhard material composite sheet.
2. The method for loading and synthesizing the thick-layer superhard material composite sheet according to claim 1, wherein: the superhard powder is one or two of diamond and cubic boron nitride.
3. The method for loading and synthesizing the thick-layer superhard material composite sheet according to claim 1, wherein: the powder used as the catalyst and the binder is one or two of cobalt powder and tantalum powder.
4. The method for loading and synthesizing the thick-layer superhard material composite sheet according to claim 1, wherein: the metal cup is a tantalum cup, a niobium cup, a zirconium cup or a molybdenum cup, and the cup cover of the metal cup is a tantalum cover, a niobium cover, a zirconium cover or a molybdenum cover.
5. The method for loading and synthesizing the thick-layer superhard material composite sheet according to claim 1, wherein: in the step (3), the compacting is performed in a compacting die at a pressure of 3 to 5 tons.
6. The method for loading and synthesizing the thick-layer superhard material composite sheet according to claim 1, wherein: in step (4), at 10 -2 ~10 -5 And (3) carrying out high-temperature purification and shaping at 600-1100 ℃ in Pa vacuum environment for 1-3 hours.
7. The method for loading and synthesizing the thick-layer superhard material composite sheet according to claim 1, wherein: in the step (5), the conditions of high-temperature high-pressure synthesis are as follows: the pressure is 5.5-7.5GPa, the temperature is 1500-1800 ℃, and the heat preservation time is 10-20min.
8. The method for loading and synthesizing the thick-layer superhard material composite sheet according to claim 1, wherein: in the step (3), at least one pre-assembled composite sheet wrapped by a metal foil is placed in a compacting die, and the metal foil outside each pre-assembled composite sheet is wrapped by pressure transmitting powder, and meanwhile each pre-assembled composite sheet is compacted.
CN202311244177.1A 2023-09-25 2023-09-25 Method for filling and synthesizing thick-layer superhard material composite sheet Pending CN117245094A (en)

Priority Applications (1)

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CN202311244177.1A CN117245094A (en) 2023-09-25 2023-09-25 Method for filling and synthesizing thick-layer superhard material composite sheet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311244177.1A CN117245094A (en) 2023-09-25 2023-09-25 Method for filling and synthesizing thick-layer superhard material composite sheet

Publications (1)

Publication Number Publication Date
CN117245094A true CN117245094A (en) 2023-12-19

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Country Status (1)

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