CN105256290B - A kind of novel diamond plating technic applied to stone cutter tool - Google Patents
A kind of novel diamond plating technic applied to stone cutter tool Download PDFInfo
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- CN105256290B CN105256290B CN201510643288.9A CN201510643288A CN105256290B CN 105256290 B CN105256290 B CN 105256290B CN 201510643288 A CN201510643288 A CN 201510643288A CN 105256290 B CN105256290 B CN 105256290B
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Abstract
The invention provides a kind of novel diamond plating technic applied to stone cutter tool, belong to diamond surface metal plating layer technical field of film preparation.Of the invention continuity containing Tungsten Carbide Thin Film and uniformity as obtained by low-temperature pressure plating and high-temperature heat treatment process is preferable, regular shape and film thickness is controllable, improves diamond caking property and high-temperature corrosion-resistance ability.Manufactured cutter its life-span and efficiency in cutting stone material are largely increased, and reduce consumption and loss.Its preparation method is simple, cost is cheap, it is easy to accomplish large-scale production.
Description
Technical field
The invention belongs to diamond surface metal plating layer technical field of film preparation, more particularly to a kind of diamond surface
Hydro-thermal plates tungsten metal layer preparation technology.
Background technology
Diamond is in itself except with excellent properties such as high, the anticorrosive, wearabilities of hardness, also with excellent optics, sound
The properties such as, calorifics and electricity.Since over half a century, the production of diamond and the development of application technology are advanced by leaps and bounds,
It has met or exceeded natural diamond in quantity, quality and many performances.Diamond and its product not only extensively should
For machinery, it is metallurgical, build each industrial technical field such as work, traffic, national defence, be extended to high performance heat-resistant piece, anti-corrosion
The key areas such as part, heat conducting element and chip.Superhard material based on diamond etc. is as the basic of Modern Manufacturing Technology
Means, support and facilitation are played to state-owned pillar industry and national defense industry.Counted according to external authoritative sources, world's diamond
Demand be just incremented by with average 8% or so annual growth rate, carbonado 50% or so is used to manufacture processing of stone work at present
Tool, wherein mainly stone material saw.It is contemplated that after diamond product is popularized, the material progress of the mankind will more last layer
Building, so peak, into the eternal diamond epoch.
At present, diamond sawing and rig instrument use powder metallurgic method production, and sintering temperature is generally up to 900 DEG C.
Under normal temperature and pressure, diamond is inferior stable state, and its heat resistance is not high.When diamond is heated to 700 DEG C or so in atmosphere,
Start oxidation weight loss phenomenon occur, anti-pressure ability declines；Graphitization phenomenon can occur for diamond more than 1000 DEG C.These phenomenons
The processing efficiency of instrument can be reduced, influences using effect.In addition, between the material interface such as diamond and most of metal, ceramics
Performance difference is larger, and interface can be higher so that be difficult to effectively soak between diamond and metal or alloy, interface binding power compared with
It is usually cast setting between difference, i.e. diamond abrasive grain and bonding agent, is easily come off in the presence of grinding force, reduce grinding tool
Service life.It is estimated that diamond utilization rate is only 60% or so in diamond impregnated tools, there are millions of carats every year
Expensive diamond drop-off and be lost among scrap, lose in terms of ten million yuan.Therefore, how to improve diamond inoxidizability,
Prevent diamond graphitization at high temperature, reduce diamond using when come off, turn into and improve diamond tool service life
Key factor.At present, it is general both at home and abroad to reduce diamond and matrix using in the method for diamond surface metal lining
Interface energy, and stable enhanced primary treatment is formed by this layer of metal and bonding agent.
Early in the early 1980s, the country goes to the fieldworker of Britain, Ireland, former West Germany just to have been found that above-mentioned country
The diamond through coating surface used accounts for more than the 80% of binding agent diamond tool production dosage, and use is through coating surface
The diamond of metalized improves the service life of instrument 30% ~ 40%, and can reduce by 20% diamond concentration.The U.S., day
This grade state uses the diamond abrasive handled through surface metallizationization compared with attention, and has accounted for significant proportion.The seventies country
Had begun to the research of diamond surface metal lining, such as diamond surface coat Cu, Ni, Co, Fe, Ni-Mo, Ni-Zr,
The metals such as Fe-Co, Co-W and alloy.But diamond surface metal lining also be there are problems that, such as coating and diamond surface knot
Close it is faint, can be peeled off in general mechanical friction；Surface Welding at High Temperature or it is powder metallurgy sintered during, exposed diamond table
Face does not have solderability still.
The precondition of diamond and metallic bond metallurgical binding be must make diamond surface epitaxial growth one uniformly,
Continuously, frivolous carbide lamella, this process need certain time, temperature, and can not be with the presence of graphite element.In bonding agent directly
Add carbide former and carry out vacuum liquid-phase sintering not only process conditions harshness, its performance is also poor, is not suitable for extensive
Industrialized production.Therefore before sintering, the diamond for manufacturing surface metalation first is coating surface Ti, V, Cr, Mo, Nb, W
And the diamond of alloy is very important.During plating, diamond table is made under certain vacuum, temperature, time conditions
The carbide lamella of one layer of controllable thickness of face epitaxial growth, coating is set to produce chemical bonding after being plated with diamond.Produced as centre
Product, the coat of metal and bonding agent carcass can be smoothly realized after short time hot pressed sintering with coated diamond and bonding agent
Between soldering combine, the metallurgical binding being also achieved that between diamond and bonding agent.Diamond surface metal liningization is just
That diamond crystal surface carbon atom acts on the superficial layer to be formed with metallurgical binding, metallic character by surface chemistry, it with
There is powerful adhesion between diamond without being peeled off by common mechanical friction.On the one hand carbide exists with diamond surface
Preferably chemical bonding, on the other hand has protective action again, and isolation is directly contacted with oxygen, prevented under diamond high temperature by oxygen
Change, and flat appearance is smooth, more attractive in appearance.
In order to obtain preferable diamond surface metal. plating layer, a variety of methods can be used, as chemical plating and plating are tied
The methods of legal, vacuum plating method, salt bath plating method, the plating of physical vacuum gas phase and physical chemistry gas phase are plated, but these coating methods are general
All over there is plating is uneven, coating layer is combined with diamond that insecure, single plating amount is low, plated thickness is difficult to control, into
The problems such as this is higher.Wherein, the micro- evaporation plating method of the vacuum of University On The Mountain Of Swallows's exploitation can realize the mistake of as little as 650 DEG C of metal lining
Journey, but atoms permeating is limited in one's ability at low temperature, and it is relatively thin to form coating, it is difficult to and satisfaction is actually needed.Hydro-thermal composite depositing process is real
Showed low temperature plating, high-temperature heat treatment diamond surface formed carbide, enhancing with diamond bond strength while, also
Damage and oxidation of the high temperature to diamond can be prevented.This technique can utilize pressure caused by the closed space of reactor, low temperature
Under in diamond surface form metal. plating layer uniform and stable, that thickness is controllable；This coating layer at high temperature with diamond
The carbide that is formed of carbon and while increase its bond strength, can effectively prevent damage and graphitization mistake of the air to diamond
Journey, and working condition is less demanding, it is easily operated etc., it is a kind of up-and-coming diamond surface coating method.
The content of the invention
The present invention has invented a kind of diamond surface water applied to cutter head to solve the deficiencies in the prior art
Hot dip tungsten metal layer preparation technology.
The present invention prepares diamond surface plating tungsten metal layer using hydro-thermal plating technic, with NiSO4·6H2O、NaWO4·
7H2O etc. is raw material, strictly controls the stoichiometric proportion and concentration of various raw materials, and solution is adjusted as assist medium with ammoniacal liquor etc.
PH value, with NaH2PO2·H2O is reducing agent, is operated under relatively low heating-up temperature, makes coreduction etc. occurs between raw material
Reaction, cleaned and drying, then pressurizeed through high-temperature heating, that is, obtain target product.
The step of specific preparation method of the present invention includes following order：
1. diamond pre-processes：First diamond is put into 10% NaOH solution and boils 10 min, deionized water cleaning 2 ~
3 times；Diamond is put into 10% HNO again320 ~ 30 min are boiled in solution, deionized water is cleaned 2 ~ 3 times；Then, at room temperature
Diamond is put into 30~40 min of immersion in Salt-Based Colloid Palladium.Finally, it is placed on stirring 10 appropriate in 5% NaOH solution
Min, preprocessing process are completed.
2. the configuration of hydro-thermal coating solution：A. preparing hydro-thermal plating tungsten solution mainly includes：27 g/L NiSO4·
6H2O, 30 mL/L lactic acid, 10 g/L sodium citrate, 29 g/L NaH2PO2·H2O, 2 g/L succinic acid, 30 g/L
Sodium tungstate（NaWO4·7H2O）, micro stabilizer（Thiocarbamide）, 0.5~1 g/L rare earth chloride.B. by step 1 gained Buddha's warrior attendant
Stone is put into matched somebody with somebody solution（pH=8.0）, after ultrasonic mixing, pour into reactor.
3. hydrothermal process：In drying box, reactor is heated at a temperature of 120,130 and 140 DEG C respectively, insulation 6
h。
4. by step 3 products therefrom, after cleaning-drying, that is, the diamond particles of coating surface tungsten metal layer are obtained.
5. the plating diamond particles obtained by step 4 need to be placed in vacuum high temperature furnace, protective gas is passed through, respectively at
800th, 1h is incubated at a temperature of 850 and 900 DEG C, you can obtain object.
The preparation of Salt-Based Colloid Palladium solution is by being by 0.5 g PdCl in the step 12It is dissolved in 40 mL concentrated hydrochloric acids
In, then 16 g/L SnCl is added wherein2·2H2O, 160 g/L NaCl is separately taken to dissolve in 1 L water, by two solution continuous
Stirring is lower to be mixed, and 3 h are incubated at a temperature of 50 DEG C, obtains Salt-Based Colloid Palladium solution.
The process for preparation of step 2 hydro-thermal plating tungsten solution is：27 g/L nickel sulfates being completely dissolved constantly are being stirred
Mix down, be added to containing 10 g/L sodium citrates, 30 mL/L lactic acid, 2 g/L succinic acid enveloping agent solution in, 30 g/L tungsten
Sour sodium；The 29 g/L sodium dihydrogen phosphate reducing agents that will be completely dissolved, under violent stirring, are added slowly to foregoing molten
In liquid；0.5~1 g/L rare earth chlorides are added, add thiocarbamide stabiliser solution, and pH value is adjusted to 8.0；Filtering solution.
The inventive method is simple, cost is cheap and coating layer is continuous, uniform, thickness is controllable, it is easy to accomplish large-scale production,
It is less demanding to instrument and equipment, it is easily operated, therefore this method has very extensive application prospect.
3.4 brief description of the drawings
Fig. 1 is the hydro-thermal plating tungsten metal layer diamond particles Flied emission electricity that the present invention is prepared under different hydrothermal temperatures
Sub- microscope figure
Fig. 2 is the hydro-thermal plating diamond particulate tungsten metal level EDS figures that the present invention is prepared under 130 DEG C of hydrothermal temperatures
Fig. 3 is the hydro-thermal plating tungsten carbide thin film diamond particle field emission electron that the present invention is prepared at different temperatures
Microscope figure
Fig. 4 is the hydro-thermal plating diamond granulated carbon W film XRD that the present invention is prepared at 850 DEG C
3.5 embodiment
[embodiment 1]
1. the preparation of solution：A. the preparation of Salt-Based Colloid Palladium solution is by being that 0.5 g palladium bichloride is dissolved in into 40 mL
In concentrated hydrochloric acid, then 16 g/L stannic chloride is added wherein, separately take 160 g/L sodium chloride to dissolve in 1 L water, two solution are existed
Lower mixing is stirred continuously, and 3 h are incubated at a temperature of 50 DEG C, obtains Salt-Based Colloid Palladium solution.B. hydro-thermal plating tungsten solution
Process for preparation is：By the nickel sulfate being completely dissolved in the case where being stirred continuously, it is added to containing sodium citrate, lactic acid, succinic acid complexing
In the solution of agent, appropriate sodium tungstate is dissolved in；The sodium dihydrogen phosphate reducing agent that will be completely dissolved, under violent stirring, slowly
Be added in previous solu；Rare earth chloride is added, adds stabilizer thiourea solution, and pH value is adjusted to 8.0；Filtering solution.
2. diamond pre-processes：First diamond is put into 10% sodium hydroxide solution and boils 10 min, deionized water
Cleaning 2 ~ 3 times；Diamond is put into 10% salpeter solution again and boils 20 ~ 30 min, distilled water cleans 2 ~ 3 times；Then, room
Diamond is put into 30~40 min of immersion in the made Salt-Based Colloid Palladiums of a in step 1 under temperature.Finally, it is placed on 5% sodium hydroxide
The appropriate min of stirring 10 in solution, preprocessing process are completed.
3. hydrothermal process：Step 2 gained diamond is put into the solution that b in step 1 matches somebody with somebody pH=8.0, after ultrasonic mixing,
Pour into reactor, be incubated 6 h at a temperature of 120 DEG C in drying box.
4. by step 3 products therefrom, after cleaning-drying, that is, the diamond particles of coating surface tungsten metal layer are obtained, are such as schemed
Shown in 1 (a).
[embodiment 2]
Hydrothermal process：[embodiment 1] step 2 gained diamond is put into the solution that b in step 1 matches somebody with somebody pH=8.0, ultrasound
After mixing, pour into reactor, be incubated 6 h at a temperature of 130 DEG C in drying box.Other steps are identical with [embodiment 1], i.e.,
The diamond particles of coating surface tungsten metal layer are obtained, as shown in Fig. 1 (b).Its component distributing is as shown in Figure 2.
[embodiment 3]
Hydrothermal process：Step 2 gained diamond is put into b in step 1 and matches somebody with somebody the solution of pH=8.0, after ultrasonic mixing, is poured into
In reactor, 6 h are incubated at a temperature of 140 DEG C in drying box.Other steps are identical with [embodiment 1], that is, obtain coating surface
The diamond particles of tungsten metal layer, as shown in Fig. 1 (c).
[embodiment 4]
Coating surface layer pattern is carried out to Composite Coatings diamond obtained by [embodiment 1], [embodiment 2] and [embodiment 3]
Compare, obtain hydrothermal temperature as 130 DEG C, when soaking time is 6 h, plating effect is best, can be as heat treatment experiment thereafter
Sample.
The plating diamond particles obtained under 130 DEG C, 6 h are placed in vacuum high temperature furnace, are passed through protective gas,
850th, 1h is incubated at a temperature of 900 DEG C, you can obtain the plating diamond particles as shown in Fig. 3 (a), (b).Its XRD such as Fig. 4 institutes
Show.
Claims (3)
1. a kind of diamond surface hydro-thermal plates tungsten metal layer preparation technology, the technique is included following steps in sequence：
A. it is as follows that oil removing, roughening, sensitization and activation and reduction, concrete operations are carried out to diamond：
Diamond pre-processes：First diamond is put into 10% NaOH solution and boils 10min, deionized water is cleaned 2~3 times；Again
Diamond is put into 10% HNO320~30min is boiled in solution, deionized water is cleaned 2~3 times；Then, at room temperature by Buddha's warrior attendant
Stone is put into 30~40min of immersion in Salt-Based Colloid Palladium.Finally, stirring 10min appropriate in 5% NaOH solution is placed on, is pre-processed
Process is completed；B. hydro-thermal plating solution is prepared：By the nickel sulfate being completely dissolved in the case where being stirred continuously, it is added to containing sodium citrate, breast
Acid, succinic acid enveloping agent solution in and add sodium tungstate；The reducing agent sodium dihydrogen phosphate that will be completely dissolved, is stirred in violent
Mix down, be added slowly in previous solu；Rare earth chloride is added, adds stabilizer thiourea solution, and adjusted pH value with ammoniacal liquor
To 8.0；Filtering solution；
Matched somebody with somebody solution is heated to 85~95 DEG C, and carries out medium speed engine tool stirring；
C. after diamond obtained by step a is sufficiently mixed with step b resulting solutions, it is put into reactor, respectively in drying box
120th, 6h is incubated at a temperature of 130,140 DEG C；
D. by step c gains, after cleaning-drying, that is, the diamond particles of the compound metal cladding of surface tungsten are obtained；
E. by step d gains, it is placed in vacuum high temperature furnace, is passed through protective gas, at a temperature of 800,850 and 900 DEG C
It is incubated 1h, you can obtain the diamond particles of the coating of Composite Coatings containing tungsten carbide.
2. the preparation technology of diamond surface hydro-thermal plating tungsten metal layer as claimed in claim 1, it is characterised in that：Step a institutes
After diamond and step b resulting solutions be sufficiently mixed, be put into reactor, 90% amount of solution kept, respectively in drying box
120th, 6h is incubated at a temperature of 130 and 140 DEG C.
3. the preparation technology of diamond surface hydro-thermal Composite Coatings titanium coating as claimed in claim 1, it is characterised in that：Step
Plating diamond particles obtained by c and d need to be placed in high temperature process furnances, be passed through protective gas, respectively at 800,850 and 900 DEG C
At a temperature of be incubated 1h.
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