CN101773807B - Method for preparing multifunctional polycrystalline diamond compact - Google Patents
Method for preparing multifunctional polycrystalline diamond compact Download PDFInfo
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- CN101773807B CN101773807B CN2009102734314A CN200910273431A CN101773807B CN 101773807 B CN101773807 B CN 101773807B CN 2009102734314 A CN2009102734314 A CN 2009102734314A CN 200910273431 A CN200910273431 A CN 200910273431A CN 101773807 B CN101773807 B CN 101773807B
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Abstract
The invention relates to a method for preparing a multifunctional polycrystalline diamond compact. The nanocatalysis and high-pressure and high-temperature gradient synthesis technology is adopted, each particle size composition of the raw diamond and the catalyzing and synthesizing process are adjusted, the microstructure and the composition of the polycrystalline diamond compact (PDC) are controlled, the functions of the PDC are controlled and optimized, and the PDC is further finely divided into an anti-shock type, an anti-wear type and a high-temperature resistance type in property to obtain three functional PDCs, thereby finely dividing the functions of the traditional market products and satisfying the functional requirements of the drilling tool cutting teeth on different working conditions and geological microenvironments. The strata adaptability and the performance-price ratio of the drill bit can be obviously enhanced, the drilling efficiency and the service life of the drill bit are reasonably balanced, the PDC property can be fully exerted, and the resource of hard alloy is saved.
Description
Technical field
The present invention is mainly used in industries such as geology core drilling, coal mining, underground drawing-off gas, natural gas and oil exploitation, engineering tools, gem processing, automobile and the processing of Aero-Space parts, is specifically related to a kind of preparation method of multifunctional polycrystalline diamond compact of high-performance and low-cost.
Background technology
Composite polycrystal-diamond (PDC) is as the critical component of drill and petroleum extraction tools, and its performance and function have determined the quality and the work efficiency of drill and petroleum extraction tools.At present, the general performance of estimating PDC from hear resistance, wearability and impact resistance three aspects.From technical standpoint, the impact resistance of PDC and wearability are what to restrict with contradiction each other under certain technical conditions, and various mining drill bit PDC cutting teeths at present are owing to cost and technical limitations.Performance is low, function singleness; Oil, has reached the balance of the two preferably with high production cost and technology, but has limited PDC in low-cost and high-performance demand market, the development in particularly general mining drill and petroleum extraction tools market as high-end product with PDC.Accept even price is market, also have the waste of some functions, and the high impact resistance that other functions such as anchor bit require can not satisfy operating mode drilling-production equipment and the geological prospecting and the drilling condition in some collieries.
PDC market mainly is to be divided into plain edition, reinforced by the polycrystalline diamond layer caliper zones both at home and abroad at present, does not see the product that segments by its functional characteristics.The multifunctional polycrystalline diamond compact that the present invention proposes is not seen domestic and foreign literature and patent report as yet.
Summary of the invention
Purpose of the present invention is low in order to overcome common PDC performance, oil PDC cost height, the shortcoming that resource requirement is high, on common PDC production technology basis, has the method for the Multifunction type composite polycrystal-diamond of multi-functional characteristic and provide a kind of by meticulous control formula for a product and the preparation of production technology regulation and control PDC performance, the present invention mainly is at the stressed difference of drill bit different parts and the different of microenvironment of working, at pressure 5.5-6.0GPa, temperature 1450-1650 ℃, adopt nano-catalytic and high pressure-temperature gradient synthetic technology, by forming the polycrystalline diamond layer of the synthetic carbon-carbon bond combination of chemical potential and temperature gradient, further micro-structural and the composition of PDC are regulated and control by adjusting prescription and catalysis and synthesis technique, realize multi-functional regulation and control of PDC composite sheet and optimization, on performance, further PDC is subdivided into the shock resistance type, wear-resisting type and high temperature resistant type three classes, to obtain three kinds of Mobyneb PDC, realization is carried out the function segmentation to existing market product, satisfies the functional requirement of drill and petroleum extraction tools cutting teeth to different operating modes and geology microenvironment.Can significantly improve the ground adaptability and the cost performance of drill bit, make drilling efficiency and bit life obtain more reasonable taking into account, better bring into play the performance of PDC, save the carbide alloy resource.The cutter that also can be used for simultaneously Digit Control Machine Tool.
Multifunctional polycrystalline diamond compact can be divided three classes by its functional characteristics:
1, the preparation method of wear-resisting type composite polycrystal-diamond, the diamond particle diameter is represented with W60 for 60 microns, the diamond particle diameter is represented with W30 for 30 microns, the diamond particle diameter is represented with W10 for 10 microns, three kinds of diamond particle diameter consumptions by weight percentage, W60 is 15-30%, W30 is 30%～50%, W10 is 20%～45%, the mass percent that the nano-cobalt powder of interpolation graphite parcel accounts for the diamond total amount is 4%～12%, by above-mentioned each material and the consumption got,, mix and place vacuum drying chamber 80-100 ℃ preservation is standby down the nano-cobalt powder and the diadust ball milling of graphite parcel 300-900 minute; Take by weighing above-mentioned diadust that mixes of 0.5-2.0g and hard alloy substrate compacting assembling and be placed in the synthetic mould of pyrophillite, put into the cubic apparatus diamond press; At pressure 5.5GPa, temperature 1400-1550 ℃, synthetic 5-15 minute, take out sample after the release, obtain the wear-resisting type composite polycrystal-diamond through mechanical polishing.Diamond layer thickness is greater than 1.5mm, and heat resisting temperature is not less than 800 ℃, cutting SiC emery wheel wear resistance ratio about 2,000,000.
2, the preparation method of shock resistance type composite polycrystal-diamond, the diamond particle diameter is represented with W60 for 60 microns, the diamond particle diameter is represented with W30 for 30 microns, the diamond particle diameter is represented with W10 for 10 microns, three kinds of diamond particle diameter consumptions by weight percentage, W60 is 40-60%, W30 is 30%～50%, W10 is 0-20%, the mass percent that the nano-cobalt powder that adds the graphite parcel accounts for the diamond total amount is 6%～10% to be catalyst, by above-mentioned each material and the consumption got,, mix and place vacuum drying chamber 80-100 ℃ preservation is standby down the nano-cobalt powder and the diadust ball milling of graphite parcel 300-900 minute; Take by weighing above-mentioned diadust that mixes of 0.5-2.0g and hard alloy substrate compacting assembling and be placed in the synthetic mould of pyrophillite, put into the cubic apparatus diamond press; At pressure 6.0GPa, temperature 1450-1650 ℃, Synthetic 2-5 minute takes out sample after the release, obtain shock resistance type composite polycrystal-diamond through mechanical polishing.Diamond layer thickness is less than 1.2mm, and heat resisting temperature is not less than 800 ℃, cutting SiC emery wheel wear resistance ratio about 1,000,000.The loop configuration design has been adopted at the base alloy interface, can reduce because of second in alloy interface and the diamond layer mutually the coefficient of expansion to produce high thermal stress greatly concentrated.Thereby improved its shock resistance greatly.
3, the preparation method of high temperature resistant type composite polycrystal-diamond, the diamond particle diameter is represented with W60 for 60 microns, the diamond particle diameter is represented with W30 for 30 microns, the diamond particle diameter is represented with W10 for 10 microns, three kinds of diamond particle diameter consumptions by weight percentage, W60 is 20-40%, W30 is 35%～55%, W10 is 10%～30%, nano SiC 4-10%, the mass percent that accounts for the diamond total amount with the nano-cobalt powder of graphite parcel is 4～6% to be catalyst, by above-mentioned each material and the consumption got, nano-cobalt powder with the graphite parcel, nano SiC and diadust ball milling 300-900 minute mix the placement vacuum drying chamber and preserve standby down for 80-100 ℃; Take by weighing above-mentioned diadust that mixes of 0.5-2.0g and hard alloy substrate compacting assembling and be placed in the synthetic mould of pyrophillite, put into the cubic apparatus diamond press; At pressure 5.5GPa, temperature 1400-1550 ℃, synthetic 5-15 minute, take out sample after the release, obtain the high temperature resistant type composite polycrystal-diamond through mechanical polishing.Diamond layer thickness is greater than 1.5mm, and heat resisting temperature is not less than 850 ℃, cutting SiC emery wheel wear resistance ratio about 2,000,000.Be to be specifically designed to the rock stratum that the hard and compact difficulty is crept into, as quartzy fine sand rock stratum, because of the fine and close abrasiveness in rock stratum is strong, temperature arrising caused by friction height, general PDC non-refractory are easy to generate thermal expansion stress and tipping or throw off with matrix.
Diamond is common high-purity bortz powder, high strength diamond powder and/or boric diamond powder.Commercially available.Central-South diamond industrial group and the Yellow River whirlwind group company buy from Henan.
The present invention mainly is at the stressed difference of drill bit different parts and the different of microenvironment of working, by adjusting prescription and catalysis and synthesis technique micro-structural and the composition of PDC are regulated and control, realize the regulation and control and the optimization of PDC composite sheet function, on performance, further PDC is subdivided into shock resistance type, wear-resisting type and high temperature resistant type three classes, to obtain three kinds of functional form PDC, realization is carried out the function segmentation to existing market product, satisfies the functional requirement of drill and petroleum extraction tools cutting teeth to different operating modes and geology microenvironment.Can significantly improve the ground adaptability and the cost performance of drill bit, make drilling efficiency and bit life obtain more reasonable taking into account, better bring into play the performance of PDC, save the carbide alloy resource.
Description of drawings
Fig. 1 is the differential thermal analysis curve figure of embodiment 3 samples.
Fig. 2 a is the shock resistance type PDC microstructure of embodiment 4 scanning electron microscope analysis.
Fig. 2 b is embodiment 3 high temperature resistant type PDC microstructures.
Fig. 3 is the nanometer cobalt TEM photo of homemade graphite parcel.
The specific embodiment
The enforcement of Mobyneb composite sheet relates to synthesis technique, prescription and substrate grooved three's coupling.
1. synthesis device and technology: equipment: cubic apparatus diamond press.Technology: utilize the cobalt diffusion of alloy substrate and the nano-cobalt powder of graphite parcel to be catalyst, at pressure 5.5-6.0GPa, by forming the polycrystalline diamond layer of the synthetic carbon-carbon bond combination of chemical potential and temperature gradient.Generated time and temperature and pressure matching technique have following dual mode.
A, 5-15 minute low temperature long period are synthesized pressure 5.5GPa among the embodiment, temperature 1400-1550 ℃; For example synthetic wear-resisting type and high temperature resistant type PDC.
B, the quick 2-5 of high temperature minute synthetic, pressure 6.0GPa among the embodiment, temperature 1450-1650 ℃; For example synthetic shock resistance type PDC.
2. material and prescription:
Diamond: common high-purity bortz powder, high strength diamond powder, boric diamond powder.Commercially available, Central-South diamond industrial group and the Yellow River whirlwind group company buy from Henan.
Granularity: adopt at least three kinds of different grain sizes, be respectively 60 microns of particle diameters among the embodiment, 30 microns and 10 microns is W60, W30, W10.
Cobalt powder: graphite parcel nano-cobalt powder, self-control, granularity 5-20 nanometer, its microstructure is seen the high resolution electron microscopy photo of accompanying drawing 3, mainly as the diamond catalyst of crystalline growth again.The preparation method of graphite parcel nanometer cobalt is as follows:
1, takes by weighing 1g Co (NO
3)
2.6H
2O, 0.6g NaOH gets 60ml ethylene glycol with pipette, and it is mixed in the beaker;
2, mixed solution was stirred on magnetic stirring apparatus 3 hours, and 170 ℃ of heated at constant temperature;
3, take by weighing 25g starch in beaker, add 30ml distilled water, stir;
4, above 2,3 solution that make of step are mixed in the beaker, place the ultrasonic 30min of ultrasonoscope after, air drying 24 hours; At last sample was put in 80 ℃ of baking ovens dry 12 hours;
5, above-mentioned sample is placed reduction furnace feed hydrogen reaction and obtain metallic cobalt;
Reaction control is as follows:
Heat up in ℃ 1h of room temperature → 300, insulation 1h feeds hydrogen 30ml/min;
300 ℃ → 500 ℃ insulation 1h, 5 ℃/min of programming rate;
500 ℃ → 900 ℃ insulation 4h;
900 ℃ → room temperature is cooled off naturally
6, metallic cobalt pickling: with the metallic cobalt of above-mentioned acquisition 1M HNO
3Solution soaked 4 hours, cleaned the back with distilled water and filtered evaporate to dryness, promptly obtained the nano-cobalt powder of graphite parcel, and the particle size of cobalt is the 5-20 nanometer.
Carborundum powder: SiC, purity 99%, granularity 40nm, your nano material company of effluent Nankai produces.
The concrete proportioning of three kinds of functional form PDC is seen before and is stated.
Table 1 functional form diamond proportioning and synthesis technique
The preparation method of multifunctional polycrystalline diamond compact, (1) mass fraction of each material is got by the amount in the table 1 respectively, with the nano-cobalt powder of graphite parcel and diadust ball milling 300-900 minute, mix and place vacuum drying chamber 80-100 ℃ preservation is standby down; (2) take by weighing above-mentioned diadust and the hard alloy substrate compacting assembling that 1g mixes and be placed in the synthetic mould of pyrophillite, put into the cubic apparatus diamond press; (3) according to the synthetic technological condition in the table 1, selection pressure and heating power and generated time take out sample after the release, obtain finished product through mechanical polishing.Wherein embodiment 1 synthesis condition is: at pressure 6.0GPa, and 1650 ℃ of temperature, Synthetic 2 minute; Embodiment 2 synthesis conditions are: at pressure 5.5GPa, and 1550 ℃ of temperature, synthetic 5 minutes; Embodiment 3 synthesis conditions are: at pressure 5.5GPa, and 1400 ℃ of temperature, synthetic 15 minutes; Embodiment 4 synthesis conditions are: at pressure 6.0GPa, and 1450 ℃ of temperature, synthetic 5 minutes; Embodiment 5 synthesis conditions are: at pressure 5.5GPa, and 1500 ℃ of temperature, synthetic 10 minutes.
High temperature resistant type and the shock resistance type PDC that makes of embodiment 3 and embodiment 4 comes experimental analysis below.
(1) heat resistance analysis:
Embodiment 3 samples, heating still keeps the good high-temperature abrasion resistance for 750-850 ℃ under air atmosphere, and differential thermal analysis (DTA) shows in its air the thermal decomposition initial temperature up to 862 ℃, only about 48% (see figure 1) of mass loss in the time of 1000 ℃; And its volume wear resistance ratio has also surpassed 5,000,000 during grinding superhard silicon carbide emery wheel.Directly be heated to 800 ℃ in Muffle furnace, be incubated 3 minutes, surveying its wear resistance ratio behind the air cooling not have loss substantially, and abrasion ratio is 0.97 (heat 800 ℃ and be incubated after 3 minutes the ratio of wear resistance ratio under the wear resistance ratio and normal temperature, it can reflect the heat endurance of PDC).Abrasion ratio maximum is 1, and is good more near 1 its high high-temp stability of reflection.
(2) regulating microstructure:
By adjusting PDC formula for raw stock and catalysis and synthesis technologic parameter (see before and state the summary of the invention part), can realize the particularly control of crystal boundary micro-structural and second phase composition and distribution of PDC heterogeneous microstructure, thereby strengthen different qualities and function such as high impact properties or the heat-resisting quantity etc. of PDC.Figure below is the microstructure comparison diagram of the scanning electron microscope analysis of embodiment 4 and example 3 samples.
The backscattered electron image that uses SEM to take PDC surface under the high magnification can be observed second situation that distributes mutually mutually among the PDC intuitively, and comparatively bright part correspondence is metallic bond among Fig. 2 a (example 4 in the correspondence table 1), Fig. 2 b (example 3 in the correspondence table 1).The size of its content what and distribution situation and diamond crystals, distribution and crystal boundary can directly influence the performance of PDC.Relatively the two microstructure is obviously different with Fig. 2 b for Fig. 2 a, and latter's bond content is very low, and diamond layer density is big, and hardness is higher.
The microhardness that microhardness testers are measured example 3 and example 4 is respectively 9000 and 5600kg/mm
2Aforementioned differential thermal analysis shows that also the former has higher heat decomposition temperature, heating heating peak value is 919.2 ℃ in air, therefore has higher resistance to elevated temperatures and extremely strong thermal stress resistance impact characteristics, is fit to the cutting teeth and the NC cutting tool of preparation oil and hard formation drill bit.But the latter can obtain better low temperature toughness with lower manufacturing cost, is fit to the high anchor bit of preparation impact toughness reguirements.
Claims (4)
1. the preparation method of wear-resisting type composite polycrystal-diamond, the diamond particle diameter is represented with W60 for 60 microns, the diamond particle diameter is represented with W30 for 30 microns, the diamond particle diameter is represented with W10 for 10 microns, three kinds of diamond particle diameter consumptions by weight percentage, W60 is 15-30%, W30 is 30%～50%, W10 is 20%～45%, the mass percent that the nano-cobalt powder of interpolation graphite parcel accounts for the diamond total amount is 4%～12%, by above-mentioned each material and the consumption got,, mix and place vacuum drying chamber 80-100 ℃ preservation is standby down the nano-cobalt powder and the diadust ball milling of graphite parcel 300-900 minute; Take by weighing above-mentioned diadust that mixes of 0.5-2.0g and hard alloy substrate compacting assembling and be placed in the synthetic mould of pyrophillite, put into the cubic apparatus diamond press; At pressure 5.5GPa, temperature 1400-1550 ℃, synthetic 5-15 minute, take out sample after the release, obtain the wear-resisting type composite polycrystal-diamond through mechanical polishing.
2. the preparation method of shock resistance type composite polycrystal-diamond, the diamond particle diameter is represented with W60 for 60 microns, the diamond particle diameter is represented with W30 for 30 microns, the diamond particle diameter is represented with W10 for 10 microns, three kinds of diamond particle diameter consumptions by weight percentage, W60 is 40-60%, W30 is 30%～50%, W10 is 0-20%, the mass percent that the nano-cobalt powder that adds the graphite parcel accounts for the diamond total amount is 4%～12% to be catalyst, by above-mentioned each material and the consumption got,, mix and place vacuum drying chamber 80-100 ℃ preservation is standby down the nano-cobalt powder and the diadust ball milling of graphite parcel 300-900 minute; Take by weighing above-mentioned diadust that mixes of 0.5-2.0g and hard alloy substrate compacting assembling and be placed in the synthetic mould of pyrophillite, put into the cubic apparatus diamond press; At pressure 6.0GPa, temperature 1450-1650 ℃, Synthetic 2-5 minute takes out sample after the release, obtain shock resistance type composite polycrystal-diamond through mechanical polishing.
3. the preparation method of high temperature resistant type composite polycrystal-diamond, the diamond particle diameter is represented with W60 for 60 microns, the diamond particle diameter is represented with W30 for 30 microns, the diamond particle diameter is represented with W10 for 10 microns, three kinds of diamond particle diameter consumptions by weight percentage, W60 is 20-40%, W30 is 35%～55%, W10 is 10%～30%, nano SiC 2.5-4%, the mass percent that accounts for the diamond total amount with the nano-cobalt powder of graphite parcel is 0～3% to be catalyst, by above-mentioned each material and the consumption got, nano-cobalt powder with the graphite parcel, nano SiC and diadust ball milling 300-900 minute mix the placement vacuum drying chamber and preserve standby down for 80-100 ℃; Take by weighing above-mentioned diadust that mixes of 0.5-2.0g and hard alloy substrate compacting assembling and be placed in the synthetic mould of pyrophillite, put into the cubic apparatus diamond press; At pressure 5.5GPa, temperature 1400-1550 ℃, synthetic 5-15 minute, take out sample after the release, obtain the high temperature resistant type composite polycrystal-diamond through mechanical polishing.
4. according to the preparation method of one of claim 1-3 described multifunctional polycrystalline diamond compact, diamond is common high-purity bortz powder, high strength diamond powder and/or boric diamond powder.
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| US8882869B2 (en) | 2011-03-04 | 2014-11-11 | Baker Hughes Incorporated | Methods of forming polycrystalline elements and structures formed by such methods |
| CN102794447B (en) * | 2012-06-13 | 2014-08-06 | 河南省亚龙金刚石制品有限公司 | Anti-impact diamond layer, diamond composite sheet and preparation method for diamond composite sheet |
| CN103949187B (en) * | 2014-05-14 | 2016-03-30 | 河南飞孟金刚石工业有限公司 | A kind of coarse granule polycrystalline diamond synthesis technique |
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| CN105672891A (en) * | 2016-01-15 | 2016-06-15 | 吉林大学 | High-thermal-stability polycrystalline diamond compact |
| CN105618499A (en) * | 2016-03-25 | 2016-06-01 | 河南四方达超硬材料股份有限公司 | Manufacturing method of high-strength and high-wear-resistance polycrystalline diamond wire drawing mold blank |
| CN105924205A (en) * | 2016-06-18 | 2016-09-07 | 河南黄河旋风股份有限公司 | Manufacture method of cellular-structure diamond compact |
| CN106747445B (en) * | 2016-12-06 | 2019-08-27 | 富耐克超硬材料股份有限公司 | A kind of high-performance composite polycrystal-diamond |
| CN106735252B (en) * | 2017-03-23 | 2019-02-05 | 上海昌润极锐超硬材料有限公司 | A method of manufacture boric diamond composite sheet |
| CN108161362B (en) * | 2017-12-27 | 2020-05-08 | 武汉锐特金刚石有限公司 | Polycrystalline diamond compact and manufacturing method thereof |
| CN110328372B (en) * | 2019-08-06 | 2021-07-02 | 金华中烨超硬材料有限公司 | Polycrystalline composite cutter and preparation process of polycrystalline diamond compact for 3C cutter |
| CN111852344B (en) * | 2020-07-15 | 2022-04-08 | 广东钜鑫新材料科技股份有限公司 | Polycrystalline diamond compact and preparation method thereof |
| CN113231898B (en) * | 2021-04-23 | 2022-12-27 | 西北工业大学 | Ultrasonic vibration auxiliary processing method for difficult-to-process SiCf/SiC ceramic matrix composite |
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