CN87101453A - Welding-type polycrystal composite with synthetic diamond and method for making thereof - Google Patents

Welding-type polycrystal composite with synthetic diamond and method for making thereof Download PDF

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Publication number
CN87101453A
CN87101453A CN87101453.XA CN87101453A CN87101453A CN 87101453 A CN87101453 A CN 87101453A CN 87101453 A CN87101453 A CN 87101453A CN 87101453 A CN87101453 A CN 87101453A
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welding
powder
diamond
agcu
binding agent
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CN87101453.XA
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CN1006613B (en
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张红武
王永杰
王宗烈
胡本权
张爱华
刘淑贞
潘文山
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RESEARCH INSTITUTE OF SYNTHETIC CRYSTALS
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RESEARCH INSTITUTE OF SYNTHETIC CRYSTALS
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Abstract

The present invention relates to the technical field of diamond synthesis glomerocryst composite.Composition, performance, the prescription of diamond synthesis synneusis sheet and the method for manufacturing welding-type polycrystal composite with synthetic diamond of welding-type polycrystal composite with synthetic diamond are provided.The particle size range of bortz powder that is used for the glomerocryst layer of complex is 120 #, 180 #, 240 #With 320 #, percentage composition is 85~88%, and the binding agent composition is Si, Ti, Ni, and its total amount is 12~15%, and the combination brazing metal film of employing is Ag, Cu, Ti, V, soldering vacuum 10 -4More than the torr, 780 ℃~950 ℃ of welding temperatures, at least 15 minutes weld intervals.

Description

The invention belongs to the technical field of super-hard compound material, relate in particular to the technical field of diamond composite.
At present, most of artificial dimond synneusis composite is to adopt direct composite methods preparation, two types product is arranged usually, a kind of is growth type polycrystalline diamond complex, its method for making is that graphite raw material (or adding a small amount of diamond fine powder) and catalyst mixing are placed in the carbide alloy substrate, at the synthetic required pressure of diamond, make the polycrystalline diamond complex under the temperature conditions; Another kind is a slug type polycrystalline diamond complex, and its method for making is that bortz powder and the mixing of cementing metal powder are placed in the carbide alloy substrate sintered combined forming under superhigh-temperature and-pressure.The common drawback of these two kinds of products all is when further making drilling tool or cutter, can not stand high-temperature soldering, and welding temperature must be limited in below 750 ℃.This is because carbide alloy and diamond polycrystal difference on thermal coefficient of expansion and thermal conductivity factor are very big, make the compound interface non-refractory of formed complex, if stand the high temperature more than 750 ℃, complex may suffer damage, even may cause between carbide alloy and the diamond polycrystal and disintegrate.These two kinds of products shortcoming during fabrication is that carbide alloy has accounted for a lot of spaces of high pressure chest and influenced output, and simultaneously, carbide alloy under high pressure often may produce micro-crack and complex is scrapped, and yield rate is reduced.
In order to overcome the shortcoming that exists on the said goods and the method for making thereof, we have invented a kind of diamond synthesis glomerocryst joint product and manufacture method thereof of vacuum welding type.
Though the Chinese invention patent communique discloses CNGK85100739 " novel artificial dimond synneusis-hard material composite gear ", but its specification does not disclose any technical spirit content, U.S. Pat P NO 4063909, also introduced the technology of polycrystalline diamond and carbide alloy welding, but also be to adopt the welding of HTHP welding material, there is similar shortcoming with directly compound product and method, the another kind of method that it is introduced is to make the diamond polycrystal that has the solder layer film, do not form complete complex, although this product is easy and other metallic matrix is welded into instrument, but be not suitable for using in the other occasion, vacuum coating technology is than directly being welded into complex cost height simultaneously, and it is complicated that technology is also wanted.
The present invention is: take to be suitable for the diamond polycrystal of welding process requirement, utilize the combination brazing metal, directly form product under vacuum condition.The method for preparing this product is not seen precedent in the same industry, be the form of composition, scolder of polycrystal and combined method thereof, or welding procedure all has tangible characteristics.
Product of the present invention is by diamond synthesis glomerocryst layer, combination solder layer and hard alloy layer are formed, the welding temperature of combination scolder is lower, but after welding is finished, the remelting temperature of formed solder layer but improves greatly, even still be not melted at 1200 ℃, help the further welding under the high temperature, be made into various tool.Simultaneously, to this combination solder layer, its coefficient of expansion circle is between diamond synthesis polycrystal and carbide alloy, formed the transition zone of the coefficient of expansion between the two-layer main material, the corresponding matching degree that has improved the coefficient of expansion between the complex composition, so that in further welding, can bear more than 750 ℃, even 1200 ℃ welding temperature and being damaged hardly.So product of the present invention has been widely used, also be adapted to the multiple technology of welding again, even employing also can near 1200 ℃ sintering welding.The weld strength height of this product product, the average shear intensity between the solder side surpass 15kg/mm owing to taken all factors into consideration its hardness and toughness in the composition of polycrystal, so product is used to make the geology drill bit, especially cream be the geology drill bit to cut tool suitable especially.
The diamond synthesis glomerocryst layer of product of the present invention is formed by the diamond of 85~88% various granularities with greater than 12% binding agent.The composition of diamond grain size proportion and binding agent is as shown in table 1:
The composition of table 1 diamond synthesis glomerocryst layer
Composition Granularity Percetage by weight %
Diamond synthesis 120# ≤ 20 Listed granularity in this table
180# ≤ 21 Be according to JB1182
240# ≤ 23 -71 classifications.
320# ≤ 24
Binding agent silicon ≤ 300# 9~11
Binding agent nickel ≤ 300# 1.5~2.5
The binding agent titanium ≤ 300# 0.5~1.5
The weld layer of product of the present invention is formed after soldering by the combination scolder, the combination scolder is by titanium film or vanadium film and the use of yellow gold film combinations, after welding is finished, weld layer forms TiAgCu or VAgCu, certainly on the interface that the glomerocryst layer joins, also generate CTiAgCu or CVAgCu, because C in welding process in the diamond and Ti or V effect generate TiC or VC film, this will make the weld strength of complex improve.Make up the various films in the scolder in general, its thickness can strict be controlled, and yellow gold scolder film not only can be controlled its thickness, also can select the different proportion of Ag and Cu.Generally between 0.04~0.008mm, the silver in the AgCu alloy firm and the ratio of copper can be 10: 90 to 72: 28 percentage by weights for titanium film that the present invention is selected or vanadium film, thickness, and its thickness is generally between 0.05~0.2mm.The content of titanium or vanadium reaches as high as 20% in weld layer, and the thickness of available Ti of the control of its amount and V film and the number of plies of use are controlled, and weld layer thickness is generally less than 0.5mm.Complex is made generally in the garden cylindricality, its diameter is in the scope of φ 6~φ 14mm, thickness is decided on the thickness of cemented carbide substrate material, diamond synthesis glomerocryst layer is usually between 0.5~2.5mm, the thickness of cemented carbide substrate can be determined between 3~12mm according to actual needs.The complex of manufacturing can cut into different shapes as required to be suitable for concrete purposes, as shown in Figure 1, is through being cut into fan-shaped part, (1) expression diamond synthesis glomerocryst layer, (2) expression weld layer, (3) expression hard alloy layer.The manufacture method of product of the present invention comprises the manufacturing that is suitable for the diamond synthesis polycrystal that vacuum brazing requires and the Vacuum Soldering Technology of polycrystal and carbide alloy.The composition of polycrystal should meet the listed requirement of above-mentioned table 1, and glomerocryst technology is carried out according to technique known.Before to polycrystal and carbide quartz welding, should perform every preparation according to the regulae generales of vacuum brazing, such as by the cleaning scrubbing of scolder, the quality examination of cemented carbide substrate, particularly carbide alloy is welded the inspection of the flatness of end face, flat more good more by the weldering end face, preferably can be controlled at irregularity degree below the 0.05mm, in any case must not surpass 0.1mm.Take vacuum welding; be in order to protect diamond particles and weld metal not oxidized by the air under welding temperature on the one hand; another purpose is to get rid of the capillary channel that sticks to diamond polycrystal or the air in the fine hole effectively, helps the infiltration of scolder, improves weld strength.Certainly, adopt the inert atmosphere protection welding also can, such as at N 2, He gas all can, but effect not as vacuum condition good.
During welding, to make up the scolder film places between diamond synthesis polycrystal and the carbide alloy, in welding process, the alloying of each film welding flux and welding are finished in same process and are carried out, the weld tabs placement is Ti(V in proper order)-AgCu-Ti(V)-AgCu, and Ti(V) be right after what be that synneusis sheet and AgCu be right after is the carbide alloy substrate, the quantity of weld layer can increase according to circumstances, but at least the above-mentioned number of plies should be arranged.Accompanying drawing 2 is scolder combination signals, and (1) is the diamond synthesis synneusis sheet, and (2) (4) are titanium film or vanadium film, and (3) (5) are the AgCu weld tabs, and (6) are cemented carbide substrate.The welded article that assembles is installed by the signal of Fig. 3 and places vacuum drying oven, be evacuated to 10 -4The vacuum that torr is above, with 5~15 ℃/minute speed intensification, temperature range can be determined according to actual needs then, the combination condition difference of combination solder sheet, its temperature range can change between 780 ℃~950 ℃.Be warming up to definite temperature and maintenance at least 15 minutes, generally in 45 minutes.Be cooled to room temperature with 5~15 ℃/minute speed then, in whole welding process, all should keep desired vacuum, certainly in temperature-fall period, guaranteeing that welded article does not have under the oxidized prestige association condition, but also ahead relieving vacuum state.
The production method of this product, to the eye, the product that high pressure high temperature polymeric composite of ratio forms, it is complicated that technology is wanted, it is many that step is wanted, and the cycle will be grown, but in fact, the product that is obtained has not only overcome all shortcoming of method for making products obtained therefrom in the past, and significant feature has been brought into play in the raising of productivity ratio.Because make in this way, when the preparation polycrystal, once can produce two, and yield rate is high again, when welding, once can weld some in the vacuum drying oven, output greatly improves.
The following embodiment that provides can further specify content of the present invention, concrete parameter that example proposed is the more specific of above-mentioned each process conditions, rather than limits the scope of the invention.
Example one
The mixture of forming diamond and binder material according to table 2, and abundant mixing, thickness and diameter according to required glomerocryst requirement, accurately take by weighing every deal, in vacuum drying oven, carry out purified treatment then, the compound of handling is packed in the known high-pressure bottle, is pressed into the synneusis sheet of 1mm by known high-temperature and high-pressure conditions.
The diamond of table 2 synneusis sheet and binding agent are formed
Bortz powder percentage composition % 120# 19.5 180# 20.5 240# 22 320# 23
Binding agent percentage composition % Si ≤300# 10 Ni ≤300# 2.5 Ti ≤300# 2.5
The synneusis sheet of making is handled impurity such as removing graphite with perchloric acid, clean oven dry, the hard metal tip that desire is connect is planarized to and meets welding requirements and clean in clean oven dry, with scolder film AgCu28,0.1mm and the garden sheet that the Ti0.008mm punching out becomes to be suitable for is cleaned oven dry, form by Fig. 2 fits together, and the signal by Fig. 3 is installed then, places vacuum drying oven to weld.Among Fig. 31 is hold-down screw, the 2nd, and briquetting, the 3rd, by the welded part of Fig. 2 assembling, the 4th, graphite cake 5 is base plates.
Welding condition is: be evacuated to 10 earlier -4More than the torr then the heating rate with 15 ℃/min be warming up to 830 ℃, be incubated 30 minutes, be cooled to room temperature with the speed of 15 ℃/min then and can take out product.
Example two
Form the step identical according to listed bortz powder of table 3 and binding agent and make the thick dimond synneusis sheet of 2mm with example 1, then by the listed step of example 1, replace AgCu28 with the AgCu50 weld tabs, replace the Ti0.008mm film with V0.004mm, assemble by the mode of Fig. 2 and Fig. 3 then and be installed, enter the vacuum furnace brazing, the soldering condition is to be evacuated to 10 -4More than the torr, be warming up to 950 ℃ with 5 ℃/min speed then and kept 45 minutes, be cooled to room temperature with 5 ℃/min speed then and can take out product.
The composition of table 3 bortz powder and binding agent
Bortz powder percentage composition % 120# 20 180# 21 240# 23 320# 24
Binding agent percentage composition % Si ≤300# 9.5% Ni ≤300# 2% Ti ≤300# 0.5%
*System is according to the JB1182-71 gauge.

Claims (5)

1, a kind of welding-type polycrystal composite with synthetic diamond is made up of diamond synthesis glomerocryst lamella, solder layer and hard alloy layer, it is characterized in that:
A, said diamond synthesis synneusis sheet composed as follows:
Bortz powder is between 85~88%, and the binding agent composition is that Si, Ti, Ni mix total amount between 12~15%;
B, said solder layer are to be formed by AgCu alloy weld tabs and Ti film or V film combinations, form TiAgCu or VAgCu solder layer after the vacuum welding process, and layer thickness is less than 0.5mm;
2,, it is characterized in that the bortz powder of said diamond synthesis synneusis sheet and the composition percent by weight composition of binding agent are: 120 by the product of claim 1 defined #Bortz powder≤20%, 180 #≤ 21%, 240 #Powder≤23%, 320 #Powder≤24%, the percentage composition of binding agent is :≤300 #Si powder 9~11%, Ni powder 1.5~2.5%Ti powder 0.5~1.5%.
3, according to the diamond synthesis synneusis sheet of claim 2 defined, it is characterized in that thickness is 0.5~2.5mm, diameter is at φ 6~φ 14mm.
4, a kind of manufacture method of welding-type polycrystal composite with synthetic diamond, in advance bortz powder and binding agent powder are evenly mixed, through under high-temperature and high-pressure conditions, being prepared into the alloy dimond synneusis sheet after the purified treatment, then synneusis sheet and carbide alloy substrate are made polycrystal composite with synthetic diamond by vacuum brazing, it is characterized in that:
A, bortz powder and binding agent composition were formed by table 1 when said diamond synthesis synneusis sheet prepared:
Table 1 The granularity percentage composition of bortz powder 120# ≤20% 180# ≤21% 240# ≤23% 320# ≤24% The percentage composition % of binding agent composition Si ≤300# 9~11 Ni ≤300# 1.5~2.5 Ti ≤300# 0.5~1.5
B, the employed scolder of said vacuum brazing are a kind of combination scolders of metallic film, and they are made up of AgCu weld tabs and Ti film or V film; The combination scolder is in welding process, and alloying and welding are finished simultaneously.
C, said vacuum brazing require 10 -4The vacuum condition that torr is above, welding temperature is between 780 °~950 ℃, and temperature rate is 5 °~15 ℃/minute, and welding was held time 15 minutes at least;
5, according to the method for claim 4 defined, the metallic film Ti or the V that it is characterized in that said combination scolder are that 0.008~0.04mm is thick, the thickness of AgCu alloy sheet is at 0.05~0.2mm, Ag: Cu was from 10: 90~72: 28, each sheet built-up sequence is that Ti or V-AgCu-Ti or V-AgCu two are respectively alloy dimond synneusis sheet and carbide alloy substrate, the number of plies of combination scolder film and every thickness thereof is on deciding welding requirements, but should comprise four layers of following order at least: Ti(V)-AgCu-Ti(V)-and AgCu.
CN 87101453 1987-11-28 1987-11-28 Welding-type polycrystal composite with synthetic diamond and its manufacturing method Expired CN1006613B (en)

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CN100368140C (en) * 2004-06-03 2008-02-13 吉林大学 Method for connecting diamond thick film with hard base firmly
CN101940894A (en) * 2010-10-28 2011-01-12 郑州三和金刚石有限公司 Method for machining elliptic polycrystalline diamond for drilling
CN103121673A (en) * 2013-02-06 2013-05-29 燕山大学 Method for preparing diamond sintered body by using discharge plasmas in sintering mode
CN103658769A (en) * 2012-09-26 2014-03-26 深圳市中天精密工具有限公司 Polycrystalline diamond drill bit and manufacturing method thereof
CN103894695A (en) * 2014-04-22 2014-07-02 太原理工大学 Method for welding CVD diamond thick film and hard alloy
CN110394521A (en) * 2019-08-02 2019-11-01 太原理工大学 Diamond film high efficiency and heat radiation material and preparation method thereof
CN110983143A (en) * 2019-04-08 2020-04-10 成都惠灵丰金刚石钻头有限公司 PDC matrix drill bit powder formula
CN118218921A (en) * 2024-05-24 2024-06-21 吉林大学 Manufacturing method of diamond compact with L-shaped alloy substrate

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100368140C (en) * 2004-06-03 2008-02-13 吉林大学 Method for connecting diamond thick film with hard base firmly
CN101940894A (en) * 2010-10-28 2011-01-12 郑州三和金刚石有限公司 Method for machining elliptic polycrystalline diamond for drilling
CN101940894B (en) * 2010-10-28 2012-09-19 郑州三和金刚石有限公司 Method for machining elliptic polycrystalline diamond for drilling
CN103658769B (en) * 2012-09-26 2016-12-07 深圳市中天精密工具有限公司 Polycrystalline diamond compact bit and manufacture method thereof
CN103658769A (en) * 2012-09-26 2014-03-26 深圳市中天精密工具有限公司 Polycrystalline diamond drill bit and manufacturing method thereof
CN103121673B (en) * 2013-02-06 2015-11-18 燕山大学 A kind of discharge plasma sintering prepares the method for diamond sinter
CN103121673A (en) * 2013-02-06 2013-05-29 燕山大学 Method for preparing diamond sintered body by using discharge plasmas in sintering mode
CN103894695A (en) * 2014-04-22 2014-07-02 太原理工大学 Method for welding CVD diamond thick film and hard alloy
CN103894695B (en) * 2014-04-22 2015-12-09 太原理工大学 The welding method of a kind of cvd diamond thick film and carbide alloy
CN110983143A (en) * 2019-04-08 2020-04-10 成都惠灵丰金刚石钻头有限公司 PDC matrix drill bit powder formula
CN110394521A (en) * 2019-08-02 2019-11-01 太原理工大学 Diamond film high efficiency and heat radiation material and preparation method thereof
CN110394521B (en) * 2019-08-02 2021-03-23 太原理工大学 Diamond film high-efficiency heat dissipation material and preparation method thereof
CN118218921A (en) * 2024-05-24 2024-06-21 吉林大学 Manufacturing method of diamond compact with L-shaped alloy substrate

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