CN1433862A - Method for preparing composition gradient intermediate transition layer on wedge shape or complex shape drill working-surface - Google Patents
Method for preparing composition gradient intermediate transition layer on wedge shape or complex shape drill working-surface Download PDFInfo
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- CN1433862A CN1433862A CN 03118704 CN03118704A CN1433862A CN 1433862 A CN1433862 A CN 1433862A CN 03118704 CN03118704 CN 03118704 CN 03118704 A CN03118704 A CN 03118704A CN 1433862 A CN1433862 A CN 1433862A
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Abstract
The method for preparing interediate transition layer with component gradient change in the molybdenum sleeve of wedge of complex form hand alloy drill bit PCD job by adopting two-step operation process is characterized by that its method includes the following two steps: (1). in the sleeve, pre-adopting wear-resistant coating layer dried powder conglobation granules to press out gravured female die; and (2). in the dried powder gravured female die injecting suspension slurry for several times by leyers, drying so as to form the invented intermediate transion layer with component gradient changed structure. The combination of the above-mentioned two-step processes can prepare the polycrystal diamond strengthened wedge composite tooth with intermediate transion layer, its impact resistance is greater than 400 joules.
Description
Technical field
The present invention relates to prepare the technology of diamond-carbide alloy intermediate layer that the composition gradient transition changes at wedge shape or complicated shape drill bit working surface, be particularly related to and adopt liquid-phase precipitation dry powder absorption method to press the composition graded at the carbide drill working surface, layering prepares diamond-carbide alloy complex gradient transition zone technology.
Background technology
Diamond-carbide alloy on the insert bit is to be assembled on the hard-metal insert matrix by diadust other fortification substance raw materials that mix, by the synthetic diamond bonding of high temperature and high pressure method is main even polycrystalline diamond (PCD), realizes the composite teeth of diamond layer and matrix carbide alloy metallurgical binding simultaneously.
Because the carbide alloy of elastic modelling quantity, thermal coefficient of expansion and the matrix of PCD differs bigger, the preparation process of process HTHP greatly reduces the impact resistance of composite teeth existing at the interface up to the residual stress about 1.5Gpa.Statistics shows, in the process of deep-well construction, the crash rate of PCD drill bit is to come off from matrix owing to shock resistance difference causes diamond layer up to 1/3rd situation, therefore reduce residual stress, improve impact resistance to prolonging bit life, it is significant improving drilling efficiency, adopt compound transition zone technology that the polycrystalline diamond layer composition is changed successively, physical property also gradually changes, and can reach like this to reduce the part residual stress, improves the purpose of composite teeth impact resistance.
The intermediate layer preparation of composite teeth, usually adopt the powder carvel built, but this method only is fit to plane teeth surface simple in structure, prepare the transition zone of composition graded in comparatively complicated bit face, only introduce to some extent in the U.S., Muscovite patented technology, they generally adopt high-strength organic binder bond material requested to be prepared into the band of plastically deformable, through rolling repeatedly, after increasing compactness, be modified to suitable cemented carbide with complicated shape bit face shape, assemble at last.Adopt this method need revise ribbon shape, it is comparatively suitable to be used for axisymmetric hemi-spherical ended shape insert, and for comparatively complicated or special shape, easily produce in the band junction repeat to fold, uneven thickness, band need high pliability just easily folding, thereby need to add the organics additive of more amount, generally be higher than 20%, the high-load organics additive is easy to high residue, and may influence to some extent the composite teeth performance.
Summary of the invention
The purpose of this invention is to provide a kind of being suitable at the wedge shape or the carbide drill working surface of complicated shape more, preparation has the method for diamond-hard alloy layer that composition gradient changes.
Intermediate layer preparation technology of the present invention adopts gradient layer layering preparation, the outermost layer raw material adopts the reunion powder compacting, intermediate layer then utilizes suspension slip-casting technology natural subsidence to form, it promptly is the organic binder bond that is lower than weight 5% by admixture in powder stock, through the wear-resisting dry powder layer of mixing and compound composition, with the composite suspension liquid powder layer of individual layer composition gradient transition, through two step method preparation technology, mutual adsorption and diffusion, infiltration and realizing.
Be to realize the object of the invention, propose a kind of method step for preparing the composition gradient intermediate layer at wedge shape or complicated shape drill bit working surface and be:
1), in drill bit working surface molybdenum jacket former, compound reunion powder and the dry-pressing of adopting bortz powder and cobalt powder adding additives evenly to be mixed with go out the planar impression of recessed former drill bit work, there is the dry powder mould of impression dry under vacuum this, forms the outermost layer wearing layer that coincide with drill bit working surface shape together with molybdenum jacket former;
2), intermediate layer individual layer proportioning components by design takes by weighing bortz powder, the WC powder, cobalt powder or molybdenum powder, after titanium valve and rare earth material micro mist mix, make water content 35%～70% suspension with the distilled water that contains binding agent or deionized water or ethanol water, this suspension is injected in (1) the dry powder mould that impression is arranged in step, natural subsidence is adsorbed on outermost layer (wearing layer) inwall under the gravity effect, after drying, be pressed into drill bit, promptly be prepared into drill bit working surface composition gradient transition zone, multilayer transition layer if desired, taking out drill bit again carries out successively by preceding chatting method, the drill bit workpiece that assembles is through annealing in process in following 700 ℃ of vacuum or the hydrogen, through the PCD high temperature high pressure process, promptly finish the intermediate layer preparation that composition gradient changes then.
The above-mentioned bortz powder and the reunion powder of cobalt powder are 5～20 micron diamond micro mists and 0.1～2 micron metal cobalt micro mist and binding agent, the particle that the particle diameter that is agglomerated into according to a conventional method is 100～400 microns, and the particle water content is a weight 5%～10%.
The suspension of the water content 35%～70% that above-mentioned bortz powder-charing tungsten powder-cobalt powder or molybdenum powder, titanium valve and required rare earth material micro mist are mixed and made into, be particle diameter 0.5～2 micron diamond micro mist, 0.1～1.5 micron tungsten carbide tool micro mist and 0.1～1.5 micron metallic cobalt micro mist, metal molybdenum micro mist, Titanium micro mist and the required rare earth material micro mist of crossing by the known method purified treatment, with admixture the distilled water of soluble starch and reagent polyvinyl alcohol or deionized water or ethanol water arranged and the suspension of the water content 35%～70% made.
Described binding agent is to contain the distilled water of weight 0.1～%～2% soluble starch and weight 0.2%～3% reagent polyvinyl alcohol or the aqueous solution of deionized water or ethanol.
This preparation method's concrete operations step is as follows:
One, wearing layer preparation
A, the required dry powder raw material of wearing layer is handled mixing by known manner is clean;
B, add aforesaid binding agent, dry powder is prepared into wet weight 5%～10% agglomerated particle by general mode, 100～400 microns of grain graininess;
C, the b agglomerated particle is placed in the molybdenum former with wedge shape or complicated shape drill bit working face outer shape for preparing in advance, it is flat gently to shake, the material plane is carved at former upper edge drill bit working face and is held in the line, other gets a profile formpiston than actual drill bit working face volume little about 10% for preparing, place in the molybdenum former dry powder, after adding end compression, take out formpiston, promptly in the molybdenum mould, form recessed cloudy trace dry powder mould;
D, recessed cloudy trace mould is connected the molybdenum mould place together in the vacuum drying chamber, in 80 ℃ of temperature, vacuumized dry 1 hour, the cooling back is standby.
Two, composition gradient changes each individual layer step of preparation process
A, composition gradient is changed each individual layer needed raw material handle,, be prepared into the unit for uniform suspension of wet weight 35%～70% respectively by layer classification by the required weighing of each individual layer composition by processes well known is clean;
B, each individual layer unit for uniform suspension is injected in the recessed cloudy trace dry powder mould of (d), every layer of single mode suspension injection rate and dry powder mould are along concordant
C, the dry powder mould that will annotate suspension slurry connect the molybdenum shell and place together in the vacuum drying chamber, vacuumize, and dry moisture content under 80 ℃ of conditions of temperature;
D, two a, two b technologies prepare the required number of plies suspension dry film that finishes to plate mark,
E, will be by the required wedge shape of processes well known cleaning or the complicated shape working face is arranged, with the supporting carbide drill of each molybdenum shell, insert in the plate mark film working chamber that has prepared the transition tunic, end compression in addition, the work drill bit of making enters working face, so far, the drill bit workpiece assembling with gradient-structure transition zone finishes.
Three, subsequent treatment process and step
The workpiece that assembling is finished places in the vacuum drying chamber, vacuumizes, and is warmed up to 80 ℃ by 1 ℃ of/minute clock rate with stove, is warmed up to 250 ℃ with 0.5 ℃ of/minute clock rate again, insulation 0.5h, and cooling is taken out sample and is put into the vacuum hydrogen furnace, 10
-2～10
-4Under the Pa vacuum condition, from room temperature to 300 ℃ with 2 ℃ of/minute intensifications, be incubated 1 hour, be warmed up to 600 ℃ with 5 ℃/minute again, be incubated 1 hour, be warmed up to 700 ℃ with 5 ℃/minute then, feed hydrogen, be incubated 1 hour, close hydrogen and vacuumize, be incubated 20 minutes, take out standby with 5 ℃ of/minute backs that cool.
Intermediate layer among the present invention is to adopt suspension slip-casting technology natural subsidence and absorbing process to form, for powder diamond, WC, the Co that prevents to mix causes inhomogeneous because of the sinking speed difference, destroy the formation of expection gradient-structure, we regulate the intermediate layer composition by suitable technological operation and distribute.For uniform ingredients after the sedimentation of assurance intermediate layer slurry, on the one hand, improve the viscosity of slurry, increase particle interphase interaction and correlation, guarantee that powder is as a whole while sedimentation absorption; On the other hand, by the yardstick control of particle, further control the sinking speed of particle, the viscosity of suspension slurry can not unrestrictedly increase, otherwise is unfavorable for sedimentation.
Intermediate layer packaging technology of the present invention can be applicable to wedge shape and other special shape drill bit, as long as conscientiously operation, the gradation weighing is qualified, and the qualification rate of moulding can be more than 90% so.Compare other intermediate layer assembly technology, this method can increase the middle transition number of plies having advantage aspect the stability, uniformity and easy to operate and the controllability that keep moulding, is fit to large-scale production.
Description of drawings
Fig. 1 is an intermediate layer assembling schematic diagram, and 1 is wearing layer among the figure, and 2 are intermediate layer suspension material, and 3 is molybdenum jacket former.
Fig. 2 is the profile of the gradient wedge shape composite teeth finished of embodiment 1 preparation, and the figure ectomesoderm is the metal molybdenum cover, middle black be the polycrystalline diamond layer that composition gradient changes, internal layer is a hard alloy substrate.The thickness of polycrystalline diamond enhancement layer covers symmetrically from tooth top portion, combines closely with matrix, because the working face of chisel teeth is around its top, thereby this thickness distribution of enhancement layer meets its operation principle.
Fig. 3 is embodiment 1 a hard alloy substrate and transition zone SEM pattern at the interface, the interface is not smooth as seen from the figure, this is because the WC in the transition zone reunites and form fluctuating with the matrix metallurgical binding, matrix surface rises and falls and has increased the contact area of carbide alloy and transition zone (enhancement layer), can improve adhesion, the part of interface grey is the Co that is enriched in the interface, it almost cuts off transition enhancement layer and matrix, this obviously can reduce the adhesion of transition enhancement layer and matrix, and the thermally-stabilised of polycrystalline diamond worked the mischief.
Fig. 4 is embodiment 1 an intermediate layer SEM pattern, and intermediate layer is made up of the reunion WC-Co particle of white and the diamond particles of black as seen from the figure.
Fig. 5 is the SEM pattern of embodiment 1 outermost layer wearing layer, and outermost layer almost completely is made up of diamond particles as seen from the figure.
The specific embodiment
Embodiment 1
The preparation of gradient wedge shape composite teeth, its preparation technology divides that composition and assembling, the vacuum annealing of the composition of preparation, wearing layer of pretreatment of raw material, organic binder bond and assembling, intermediate layer are handled, six parts of PCD HTHP sintering.Being about 0.3mm with preparation diamond enhancing layer (comprising an intermediate layer) average thickness is example, provides each layer raw material composition.
One, the preliminary treatment of raw material
1, particle diameter 5～20 μ m bortz powders clean with the wang aqueous solution chemical method, dry standby;
2, get 0.1～2 micron cobalt powder of particle diameter, at H
2Condition is handled after 1 hour standby for following 700 ℃.
3, get 0.1～2 micron WC powder of particle diameter, under the hydrogen condition 700 ℃ handle 1 hour standby.
Two, the preparation of organic adhesive agent solution
Get distilled water 300ml; adding soluble starch 1g (analyzes pure; Shanghai chemical reagents corporation); polyvinyl alcohol 4g (purity＞90.2%; Chongqing chemical reagents corporation), (100 ℃) stir solution are mixed under hydrothermal condition, make no obvious residual solids polyvinyl alcohol in the solution; obtain binding agent 200ml, cool off standby.
Three, the composition of wearing layer and assembling
1, raw material mixes and is dry: get the good diadust 0.3g of preliminary treatment, cobalt powder 0.02g, put into the dried mixing of mortar, add binder solution 0.2～0.3ml then, add the about 0.4ml of distilled water again, after blend was ground, 80 ℃ of dryings were 2～4 hours in vacuum drying chamber.Dry back agglomerated particle dry powder water content about 8%.
2, the assembling of wearing layer: 1 agglomerated particle dry powder is got portion be placed in the molybdenum cup of getting ready, the surface shake is flat, is formpiston with little wedge-shaped drill tooth, and the mixed powder in the molybdenum cup is added end compression, makes the interior dry powder of molybdenum cup become die shape wedge shape, takes out formpiston.Add man-hour, die should be smooth, and inner face does not have breakage, 1/2 place in the molybdenum cup, matrix powder upper edge.The molybdenum cup is placed in the drying box 80 ℃ of inner dryings 1～4 hour, wearing layer completion of processing.
Four, the composition of intermediate layer and assembling
1, raw material mixes: bortz powder 0.15 gram, and tungsten carbide powder 0.1 gram, cobalt powder 0.02 gram, the transition zone powder of 10 parts of total amount 2.7 grams adds dried mixing in the agate mortar, adds binding agent 1～2ml, and distilled water is an amount of, is mixed into even suspension liquid.
2, assembling and dry: with the sucking-off of suspension liquid, evenly add in the dry wearing layer of dry good matrix molybdenum cup with suction pipe.Liquid level should a little higher than wearing layer edge highest point.Then the molybdenum cup was placed 80 ℃ of dryings of vacuum drying chamber 2 hours, the multilayer intermediate layer then repeats repeatedly to pour into a mould precipitation absorption transition zone technology if desired, at last the chisel teeth of getting ready is directly added to add in the molybdenum cup to flatten, and assembling finishes.
Five, vacuum annealing is handled
The sample that assembles is inserted in the vacuum drying chamber, is raised to 80 ℃ by 1 ℃/min by room temperature,, be warmed up to 250 ℃ with 0.5 ℃/min again, insulation was cooled off after half an hour.
Sample is put into vacuum furnace, 10
-2～10
-4Pa vacuumizes under the condition, heats up with 2 ℃/min from room temperature to 300 ℃, is incubated 1 hour.Be warmed up to 600 ℃ with 5 ℃/min again, be incubated 1 hour.Feed hydrogen after being warmed up to 700 ℃ with 5 ℃/min then, be incubated 1 hour.Close hydrogen at last and vacuumize, be incubated 20 minutes, take out after cooling with 5 ℃/min.
Six, HTHP sintering
To assemble ladder and cross layer and keep about 20min down 50Kbar, 1600 ℃, promptly on hard alloy substrate, form the gradient PCD layer of composition transition, finish the preparation that gradient PCD strengthens the wedge shape composite teeth with matrix.Wedge shape or complicated shape drill bit working surface prepare composition gradient transition middle transition layer method prefabricated workpiece, its PCD high-temperature high-pressure craft condition is made a world of difference with general PCD sintering process condition, for obtaining comparatively ideal PCD result, must adjust new PCD sintering process.
Gradient chisel teeth drill bit profile such as Fig. 2 of making, hard alloy substrate and transition zone SEM pattern are at the interface seen Fig. 3, and the SEM pattern of intermediate layer is seen Fig. 4, and outermost layer wearing layer SEM pattern is seen Fig. 5.
Claims (3)
1, a kind ofly prepare the method for composition gradient intermediate layer, it is characterized in that method step is at wedge shape or complicated shape drill bit working surface:
1), in the molybdenum jacket former of drill bit working surface, compound reunion powder and the dry-pressing of adopting bortz powder and cobalt powder adding additives evenly to be mixed with go out the planar impression of recessed former drill bit work, there is the dry powder mould of impression dry under vacuum this, forms the outermost layer wearing layer that coincide with drill bit working surface shape together with molybdenum jacket former;
2), intermediate layer individual layer proportioning components by design, take by weighing bortz powder, the WC powder, cobalt powder or molybdenum powder, titanium valve and rare earth material micro mist, after the mixing, make water content 35%～70% suspension with the distilled water that contains binding agent or deionized water or ethanol water, this suspension is injected in (1) the dry powder mould that impression is arranged in step, natural subsidence is adsorbed on the outermost layer inwall under the gravity effect, after drying, be pressed into drill bit, promptly be prepared into drill bit working surface composition gradient transition zone, multilayer transition layer if desired, taking out drill bit again carries out successively by preceding chatting method, the drill bit workpiece that assembles then through the PCD high temperature high pressure process, is promptly finished the intermediate layer preparation that composition gradient changes through annealing in process in following 700 ℃ of vacuum or the hydrogen.
2, the method for claim 1, the reunion powder that it is characterized in that described bortz powder and cobalt powder is 5～20 micron diamond micro mists and 0.1～2 micron metal cobalt micro mist and binding agent, the particle that the particle diameter that is agglomerated into according to a conventional method is 100～400 microns, particle water content are weight 5%～10%.
3, the method for claim 1 is characterized in that described binding agent is to contain the distilled water of weight 0.1～%～2% soluble starch and weight 0.2%～3% reagent polyvinyl alcohol or the aqueous solution of deionized water or ethanol.
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| CN103386460A (en) * | 2013-07-22 | 2013-11-13 | 河南科技大学 | Preparation technology for gradient composite wear-resistant conical liner plate |
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| CN111940742B (en) * | 2020-08-08 | 2022-07-05 | 邹爱忠 | Preparation method of gradient hard alloy |
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