CN101899713B - Polycrystalline superhard material with gradient nano-micro structure and synthesis method thereof - Google Patents
Polycrystalline superhard material with gradient nano-micro structure and synthesis method thereof Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
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Abstract
The invention provides a polycrystalline superhard material with a gradient nano-micro structure and a synthesis method thereof. The material and the synthesis method thereof are characterized in that: (1) the material has a nano-micro structure and no obvious crystal boundary, and a component structure can be designed to be gradient; (2) interacted growth is generated among BxCyNz subcrystals which serve as an internal superhard component; (3) growth stress generated by the inconsistent crystal orientations of the subcrystals is dispersed in the nano-micro structure, so that the internal concentrated stress is not formed; (4) a material preparation method provided by the invention comprises the steps of providing a 'nano material precursor' for growing the nano-micro structure, a growing subcrystal and a nano alloy powdered catalyst for use in the growth of the subcrystals, keeping the nano activity of the nano material precursor to form a packaged growing precursor and finally, growing the polycrystalline superhard material with the gradient nano-micro structure; and (5) the polycrystalline superhard material with the gradient nano-micro structure mainly comprises the following superhard components: BxCyNz and the carbide or nitride and the like of elements such as Ti, V, Si and the like. Compared with the prior art, the polycrystalline superhard material with the gradient nano-micro structure and the synthesis method thereof realize the gradient design growth, hardness and roughness of the polycrystalline superhard material BxCyNz with the nano-micro structure by using the nano material and the nano catalyst.
Description
[technical field]
The invention relates to a kind of polycrystalline superhard material with gradient nano-micro structure and synthetic method thereof.
[background technology]
Development along with new material technology and modern manufacturing industry, especially the development of the industry such as automobile, aerospace, oil drilling, electric wire, timber and optical equipment, the base mateiral that these relevant industries not only adopt all increases substantially at aspect of performances such as hardness, wear resistance, intensity, the working accuracy of these associated materials parts is also had to requirements at the higher level simultaneously." work wish is apt to its body, must first sharpen his tools ", modern manufacturing industry, when selecting in a large number high-precision numerical control equipment, is also had higher requirement to modern tool material and tools production.
As everyone knows, diamond is the highest material of hardness of finding at present, and its thermal conductivity, wear resistance, intensity are all very high, is the first-selection of making high-performance tool material.But simple diamond single crystal material, due to reasons such as welding difficulty, processing difficulties and size are little, makes it to be used as in a large number abrasive material, makes emery wheel, bistrique and polishing preparation etc., lies down in large size tool material field.So various countries scientific circles and branch of industry all pay much attention to, target is to search out a kind of method, can realize synthetic large size, hardness is high, wear resistance good, intensity is high, compact structure, toughness might as well, can the highly polished superhard materials of polishing.
The large dimond matrix material of applying in the market, as PCD etc., during due to diamond block sintering, added more bonded metal and hard alloy particle (as U.S. Patent No. 3,745,623, UK.2,326, the disclosed methods such as 655), so just contain the metallic binding phase of a large amount of (6-20wt%) in its internal crystal structure, so the indexs such as its wear resistance, hardness, density, thermal conductivity and frictional coefficient and application performance all fail to reach desirable high-performance polycrystal diamond requirement, as typical PCD, hardness only has 50-60GPa.Hardness, intensity and toughness also need further raising.
Since the nineties, chemical Vapor deposition process (CVD) growing diamond technology has obtained large progress, at present can be at diamond thick-film (1-2mm as about in thickness) and the film of the upper growing large-area (as Φ 200mm) of certain matrix (as Si).The hardness of diamond film and purity are very high, wear resistance good, can polishing smooth finish can reach very high, thermal conductivity is better, at the aspect such as heat sink, there is good application, but the many technical contradictions that overcome of being also difficult to that exist due to CVD diamond technology itself, make CVD diamond thick-film inside have a large amount of defects (as tiny crack, hole, non-diamond equate) and growth stress, structure is inhomogeneous, thereby its intensity is very low, fragility is large, add that CVD thick film quality is unstable and thickness is also limited, therefore its application in tool material field is subject to great limitation.
Therefore a kind of " hard (hardness reach 80GPa more than) and tough " (such as sphere number of shocks reaches more than 100,000 times) is provided, structure can design (as gradient type), microtexture fine and close (as having nano-micro structure), large size polycrystalline superhard material and synthetic method thereof are real is necessary.
Synthesised polycrystalline superhard material mainly contain two kinds of methods, a kind of is CVD method, a kind of is exactly High Temperature High Pressure (HTHP) method.
CVD method growth superhard material, as materials such as polycrystalline diamond and polycrystalline cBN, purity is high, and hardness is high, but subsurface defect is many, and stress is high, and fragility is large, unstable properties, large-scale industrialization promotion has a lot of technology limitations.
HTHP method is produced polycrystalline superhard material, and technique is relatively stable, can produce by large-scale industrial, and the space that product starting material and technique can be selected is large, and HTHP implementation method is various, has important research to be worth.At starting material, growth technique, the aspect technology such as thermodynamic condition such as growth pressure temperature have breakthrough, and can synthesize the polycrystalline superhard material with new phase structure and excellent properties completely.
Carbon nanotube is since 1991 are found, and its performance and preparation technology have obtained research widely, in the ascendant.This also provides the nano-carbon material that a kind of surfactivity is very high for New Polycrystalline superhard material is synthetic.
[summary of the invention]
In order to solve the problem of polycrystalline superhard material material require " hard and tough ", the invention provides a kind of hardness high, wear resistance is good, compact structure, good toughness, the programmable polycrystalline superhard material with gradient nano-micro structure of structure and synthetic method thereof.
According to an aspect of the present invention, polycrystalline superhard material with gradient nano-micro structure comprises its main body component BxCyNz, WC, and the carbide of the element such as Ti, V, Si or nitride etc.Importantly the sub-intergranular such as its inner BxCyNz has formed interactive growth.
The sub-intergranular of the main body components such as BxCyNz has nano-micro structure, there is no obvious crystal boundary, and sub-Jingjing does not form internal stress and concentrates among being dispersed in nano-micro structure to the growth stress of inconsistent generation.
It has the critical impurities element of material impact to performances such as hardness and intensity, as iron, cobalt, nickel, silicon, titanium, vanadium etc., or its two clock, or two or more alloy, along certain design direction distribution gradient.
The method of according to another aspect of the present invention, producing above-mentioned polycrystalline superhard material with gradient nano-micro structure comprises the steps:
(1) provide pure diamond micron particle, or cBN micron particle, or the two mixing material, according to the element components of design, form BxCyNz precursor raw material.The granularity of the micron particle of the superhard component of these monocrystalline is 0.1-99 micron.
(2) provide and be selected from CNT (carbon nano-tube) (growth of CVD method), diamond and cBN micron particle (0.1-20 micron), or three's mixture, for the nano-carbon material of growing nano microstructure.
(3) provide chosen from Fe, cobalt, nickel, silicon, titanium, vanadium etc., or its two clock, or two or more alloy nano-powder, for the catalyst of sub-crystals growth.
(4) under vacuum or protective atmosphere, catalyst and nano-carbon material are mixed, compacting, moulding, and make " nano material precursor ".
(5) under vacuum and/or protective atmosphere, BxCyNz precursor raw material particle and " nano material precursor " assembling are engaged, by composite design, be packaged into block.
(6) packaged synthesizing block is carried out to High Temperature High Pressure (temperature 1600K-2200K, pressure is greater than 8GPa) and process 15-1800 second, grow into polycrystalline BxCyNz constant gradient type nano-micro structure polycrystalline superhard material.
Compare with existing prior art, applying nano carbon material of the present invention and nano-catalyst have been realized the interactive mode growth of the sub-intergranular of the superhard components such as polycrystalline BxCyNz, gained polycrystalline superhard material has nano-micro structure, and impurity and performance have the characteristic of Gradient distribution, can design.(size is little not only to have reduced the degree of lattice mismatch, the brilliant grain boundary width of son is little, the crystal face angle that interface may exist is just little, reduced lattice dislocation), and lattice mismatch region can be narrowed down to submicron to nano level, so just disperseed stress area, part has been eliminated stress concentration, thereby has reduced on the whole the internal stress of body material.
In a word, synthetic large size polycrystalline BxCyNz constant gradient type nano-micro structure polycrystalline superhard material, the brilliant purity of BxCyNz after the purity of pressure, temperature, raw material and the degree of activation of nano material etc. have determined to transform, the maintenance of the pressure and temperature after conversion is the key of sub brilliant intergrowth.
Polycrystalline superhard material with gradient nano-micro structure bulk strength of the present invention is high, and wear resistance is good, compact structure, and hardness is high, and toughness is fine.
[accompanying drawing explanation]
Fig. 1 is that the present invention is for the synthesis of the synthetic assembling of Tool in Cutting material schematic diagram;
Fig. 2 is that the present invention is for the synthetic assembling of bit cutting material schematic diagram;
Fig. 3 is that the present invention processes synthetic assembling schematic diagram for high pressure-temperature;
Fig. 4 is that the present invention is for the synthetic assembling of penetrator material schematic diagram;
Fig. 5 is the SEM photo of synthetic polycrystalline superhard material with gradient nano-micro structure polished surface of the present invention after chloroazotic acid is processed, and it shows that the sub-intergranular of BxCyNz forms intergrowth.
Fig. 6 is the SEM photo of synthetic polycrystalline superhard material with gradient nano-micro structure fracture of the present invention, and its sub-intergranular that shows the superhard components such as BxCyNz forms intergrowth.
[embodiment]
The present invention utilizes nano-carbon material, diamond and cBN micro mist and nano-catalyst material mixing, form " nano material precursor " 3, nano material precursor 3 is assembled into growth precursors again with compared with the pure diamond of coarsness 4, growth precursors is under high-temperature and high-pressure conditions, 4 interactions of " nano material precursor " and pure diamond, growth forms polycrystalline superhard material with gradient nano-micro structure.Preparation process is as follows:
(1) first prepare the standby highly purified CNT (carbon nano-tube) of CVD legal system (diameter 20-50 nanometer, long 10-500 micron), front body diamond and cBN powder (granularity 0.1-20 micron) and nano-catalyst iron powder, (0.5-1) by weight: (0.5-1): (0.5-1): ratio feeding (1-2), then after adding analytical pure ethanol, put into ball grinder, add polycrystalline diamond ball to carry out ball milling mixing (continuing 4-6 hour).
(2) while 4, two kinds of granularity 5-20 of the pure micro mist of reserve fund hard rock and 20-90 micron; The ratio proportioning that is 10: 90 in the weight ratio of 5-20 micron diamond micro mist and 20-90 micron diamond micro mist.Identical method, with the other pure micro mist 4 of ball milling jar wet ball mill Buddha's warrior attendant diamond,, abrading-ball adopts polycrystalline diamond ball.Continue 4-6 hour.
(3) the good material of ball milling is reclaimed dry, then send into vacuum flush system (not indicating) and purify, through 500-600 degree hydrogen reducing, process, insulation 30-50 minute, passes into nitrogen protection (not indicating) after cooling.And consult Fig. 1, and according to nano material precursor 3, bortz powder 4 is with (10-15) %: (90-85) part by weight of %, nano material precursor 3 is first packed in zirconium pot 2, and then pack bortz powder 4 into, reinstall WC alloy substrate 5.Finally whole synthesizing block is encapsulated in zirconium crucible 6, packs graphite pressure head 1 simultaneously into, be assembled into " growth precursors " 7.
(4) consult Fig. 3, then growth precursors 7 is inserted in heating stove 8, bell 9 beyond the Great Wall.
(5) so heating stove integral body is put into high temperature high pressure device (not indicating), at pressure, be greater than 8GPa, under temperature 1600-2200K condition, process growth 15-1800 second.
(6) growth precursors of crossing through high temperature high pressure process, through being cooled to room temperature, becomes polycrystalline superhard material with gradient nano-micro structure.
(7) optionally,, before packing alloy substrate 5 into, nano material precursor 3 and pure diamond 4 can circulate and repeatedly by different ratios, feed.Finally form growth precursors.
(8) consult Fig. 2, nano material precursor 3 also needs to be contained between alloy substrate 25 and pure diamond 4, and the ratio of the weight of nano material precursor 3 and pure diamond 4 is at (10-15): (90-85).
(9) consult Fig. 4, nano material precursor 3 can be at the center of pure diamond powder 4, and at this moment the profile of growth precursors is semisphere or other complicated shapes.
(10) optionally, nano material precursor can be encased in to any hypertrophy position of non-working surface, can grow the polycrystalline superhard material with nano-micro structure of excellent specific property.As Fig. 5, shown in Fig. 6.
Embodiment mono-:
The cutter material that lathe tool is used is done in growth: refer to Fig. 1.
Table one: the cutter material component proportion example that lathe tool is used is done in growth
According to table one, be equipped with nano material precursor, added ethanol wet ball mill 4 hours, then taken out dryly, sent into vacuum flush system (not indicating), 750K hydrogen, purifying treatment 30 minutes, passes into nitrogen after cooling, refers to Fig. 1 assemble in situ.Pressure 8GPa, under temperature 1600-2200K condition, processes growth 120 seconds, then cooling, unload pressure, obtain 14 millimeters of diameters, high 5 millimeters of gradient type nano-micro structure polycrystal.
Embodiment bis-:
The cutting material that drill bit is used is done in growth: refer to Fig. 2.
Table two: the component proportion example of bit cutting material is done in growth
According to table two, be equipped with nano material precursor, added ethanol wet ball mill 6 hours, then taken out dryly, sent into vacuum flush system (not indicating), 780K hydrogen, purifying treatment 40 minutes, passes into nitrogen after cooling, refers to Fig. 2 assemble in situ.Pressure 8GPa, under temperature 1600-2200K condition, processes growth 150 seconds, then cooling, unload pressure, obtain 14 millimeters of diameters, high 8 millimeters of gradient type nano-micro structure polycrystal.
Embodiment tri-:
The bulb material of penetrator is done in growth: refer to Fig. 1.
Table three: the bulb material component proportioning example of penetrator is done in growth
According to table three, be equipped with nano material precursor, added ethanol wet ball mill 6 hours, then taken out dryly, sent into vacuum flush system (not indicating), 760K hydrogen, purifying treatment 30 minutes, passes into nitrogen after cooling, refers to Fig. 1 assemble in situ.Pressure 8GPa, under temperature 1600-2200K condition, processes growth 25 seconds, then cooling, unload pressure, obtain 4 millimeters of diameters, high 5 millimeters of gradient type nano-micro structure polycrystal.
Claims (1)
1. a method of producing polycrystalline superhard material with gradient nano-micro structure, comprises the following steps:
(1) provide pure diamond micron particle, or cBN micron particle, or the two mixing material, according to the element components of design, forming BxCyNz precursor raw material, the granularity of the micron particle of the superhard component of these monocrystalline is 0.1-99 micron;
(2) provide the CNT (carbon nano-tube) that is selected from the growth of CVD method, the cBN micron particle of diamond and 0.1-20 micron, or three's mixture, for the nano-carbon material of growing nano microstructure;
(3) provide chosen from Fe, cobalt, nickel, silicon, titanium, vanadium, or its two kinds, or two or more alloy nano-powder, for the catalyst of sub-crystals growth;
(4) under vacuum or protective atmosphere, catalyst and nano-carbon material are mixed, compacting, moulding, and make " nano material precursor ";
(5) under vacuum and/or protective atmosphere, BxCyNz precursor raw material particle and " nano material precursor " assembling are engaged, by composite design, be packaged into block;
(6) packaged synthesizing block is carried out high temperature high pressure process 15-1800 second, temperature 1600K-2200K wherein, pressure is greater than 8GPa, grows into polycrystalline BxCyNz constant gradient type nano-micro structure polycrystalline superhard material.
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| CN106077584B (en) * | 2016-06-23 | 2018-10-09 | 奇男子五金制品（浙江）有限公司 | The preparation method of superhard wear composite blade |
| CN109369192A (en) * | 2018-11-29 | 2019-02-22 | 盐城师范学院 | A kind of preparation method of cubic boron nitride |
| CN109748276B (en) * | 2019-01-10 | 2020-12-18 | 南方科技大学 | Diamond core nano polycrystalline material, preparation method thereof and superhard cutter |
| CN112760543A (en) * | 2020-12-25 | 2021-05-07 | 四川川钨硬质合金有限公司 | High-strength and high-toughness hard alloy and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1126712A (en) * | 1994-08-29 | 1996-07-17 | 史密斯国际公司 | Whisker or fiber reinforced polycrystalline cubic boron nitride and diamond |
| CN1471567A (en) * | 2000-10-12 | 2004-01-28 | ����Ԫ��(�ع�)��˾ | Polycrystalline abrasive grit |
| CN1482275A (en) * | 2002-09-09 | 2004-03-17 | 姜福英 | Method for preparing diamond/carbon or nitride nano mix phase gradient composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1126712A (en) * | 1994-08-29 | 1996-07-17 | 史密斯国际公司 | Whisker or fiber reinforced polycrystalline cubic boron nitride and diamond |
| CN1471567A (en) * | 2000-10-12 | 2004-01-28 | ����Ԫ��(�ع�)��˾ | Polycrystalline abrasive grit |
| CN1482275A (en) * | 2002-09-09 | 2004-03-17 | 姜福英 | Method for preparing diamond/carbon or nitride nano mix phase gradient composite material |
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Denomination of invention: Polycrystalline superhard material with gradient nano-micro structure and synthesis method thereof Effective date of registration: 20150625 Granted publication date: 20140924 Pledgee: Beijing technology business factoring Ltd. Pledgor: Beijing Qingdaweina Technology Ltd. Registration number: 2015990000505 |
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Denomination of invention: Polycrystalline superhard material with gradient nano-micro structure and synthesis method thereof Effective date of registration: 20161027 Granted publication date: 20140924 Pledgee: Beijing technology business factoring Ltd. Pledgor: Beijing Qingdaweina Technology Ltd. Registration number: 2016990000911 |
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