CN107868948A - A kind of method of the chemical plating cobalt coated tungsten carbide based on cobalt salt activation - Google Patents
A kind of method of the chemical plating cobalt coated tungsten carbide based on cobalt salt activation Download PDFInfo
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- CN107868948A CN107868948A CN201711250006.4A CN201711250006A CN107868948A CN 107868948 A CN107868948 A CN 107868948A CN 201711250006 A CN201711250006 A CN 201711250006A CN 107868948 A CN107868948 A CN 107868948A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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Abstract
Soaked the invention discloses a kind of method of the chemical plating cobalt coated tungsten carbide based on cobalt salt activation, including using by macrocrystalline tungsten carbide powder in cobaltous sulfate sodium hypophosphite activating solution under the conditions of ultrasonic disperse, instead of conventional precious metal activation method；Then, the powder after immersion is being heated in batch-type furnace.Afterwards, the activation powder after heat treatment is cleaned and filtered, electroless cobalt plating is carried out after drying.Preparation process of the present invention is simple to operate, reproducible, and batch mixing and reaction are uniform, while preparation time is short, and without using heavy metal, activating solution recoverable, pollution-free, cost is low.It can be used for many aspects such as magnetic material, alloy material.
Description
Technical field
The invention belongs to Hardmetal materials preparation field, more particularly to a kind of electroless cobalt plating bag based on cobalt salt activation
The method of tungsten carbide.
Background technology
Hard alloy is passed through by the hard compounds (such as WC, TiC) and binding metal (Co, Ni etc.) of refractory metal
A kind of alloy material made of powder metallurgical technique.Hard metal article after sintered shaping not only has the height of ceramics hard
Degree, high-wear resistance and excellent red hardness and heat endurance and corrosion resistance, at the same but also with metal intensity with it is excellent
Toughness, " industrial tooth " is described as, is widely used in military project, space flight and aviation, machining, metallurgy, oil drilling, mine work
The fields such as tool, telecommunications, building, therefore, common blade of as low as living all can be seen greatly to large tunnel development machine with cutter
" figure " of hard alloy.
Hard alloy Binder Phase is that by refractory metal hard compounds (hard phase), closely bonding exists in hard carbide industry
Soft metal phase together, it is the important component of hard alloy.Iron family element Fe, Ni and Co meet conditions above, always with
To be widely used as hard alloy Binder Phase metal.Particularly Co, it is most popular a kind of bonding in current hard alloy
Phase metal.At present, in most of industrial productions, the mode of the mixing generally use mechanical mixture of hard phase and Binder Phase, machine
Tool mixes low cost, easily operated, but relatively inefficient, and mixing is uneven, can also produce impurity in the product sometimes,
The so product of sintering out is not fine and close, so as to cause the reduction of performance.Therefore, in order that Binder Phase is distributed in hard phase
Evenly, its effect has preferably been given play to, scholars start to explore new hybrid mode, and have done substantial amounts of research, chemical plating
It is exactly one of which.
A kind of patent (TiB of Sun Shuo, stone dimension2The method of powder surface palladium activation-free phosphorous-nickel alloy chemical plating:,
CN101724831A [P] .2010.) report a kind of TiB2The method of powder surface palladium activation-free phosphorous-nickel alloy chemical plating, prepare
During by by TiB2Powder carries out high-temperature process in 300-500 DEG C, to substitute precious metal palladium activation method, realizes
TiB2Powder surface carries out chemical plating nickel-phosphorus alloy；Patent (Zou Zhongli, Geng Guihong, Ma Jinfu, waits a kind of silicon carbide powders of
Palladium-free activation process:, CN104561942A [P] .2015.) and a kind of palladium-free activation process of silicon carbide powder is reported, in SiC
Powder is put into the ethanol solution of ferric nitrate and activated by powder pretreatment stage, then realizes and carries out chemistry in surface of SiC
Copper facing；(Zhu flows patent, Wang Jinfang, Tu Zhibiao, waits a kind of preparation methods of few Binder Phase Talide of:,CN
104232967 A [P] .2014.) report a kind of preparation method of few Binder Phase Talide, profit in preparation process
The activating solution formed with hydrofluoric acid, nitric acid, ammonium fluoride and hydrochloric acid carries out surface active to tungsten carbide, is then stirred in chemical plating fluid
Mix and realize tungsten carbide surface cobalt plating.Document (Guo L, Xiao L R, Zhao X J, et al.Preparation of WC/Co
composite powders by electroless plating[J].Ceramics International,2017, 43
(5):A kind of preparation method at tungsten carbide-cobalt composite powder end 4076-4082.) is reported, palladium bichloride, chlorine are utilized in preparation process
Change stannous and hydrochloric acid mixed solution and activation process carried out to tungsten carbide, after the tungsten carbide of activation process is applied in chemical plating fluid
Plating, obtain the nano-tungsten carbide powder of the uniform plating cobalt layers in surface.Although achieve very big to enter in electroless plating technology at present
Exhibition, but still suffer from the problem of certain, on the one hand, the more good precious metal activation technique cost of activation effect is too high, simultaneously
Serious pollution can be caused to environment, can not be produced on a large scale；On the other hand, some existing no-palladium activating modes will
By strong acid, high temperature or other metal salt solutions, impurity would generally be produced during chemically plating is standby, or cause the energy and environment
Burden, and activating solution less stable.
Based on it is existing the problem of, the present invention is based on chemically plating Preparation Method activate to tungsten carbide surface using cobalt salt, work
Change stage process is simple, and cost is low, and the stable reusable edible of activating solution, the electroless cobalt plating bag tungsten carbide powder prepared are equal
Even, impurity is few.At present, report is had no to the chemically plating Preparation Method that tungsten carbide surface activates based on use cobalt salt.
The content of the invention
Goal of the invention：For the present Research of Hardmetal materials, the present invention provides a kind of high evenness, pollution less and made
A kind of method of the low chemical plating cobalt coated tungsten carbide based on cobalt salt activation of standby cost.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：A kind of electroless cobalt plating based on cobalt salt activation
The method of bag tungsten carbide, comprises the following steps：
A kind of method of the chemical plating cobalt coated tungsten carbide based on cobalt salt activation, it is characterised in that comprise the following steps：
(1) tungsten carbide powder is added in hydrofluoric acid-nitric acid coarsening solution, is roughened under ultrasonic disperse effect, then filters
And dry, obtain being roughened powder；
(2) the roughening powder that step (1) obtains is added in cobaltous sulfate-sodium hypophosphite activating solution in ultrasonic disperse environment
Lower carry out immersion treatment；
(3) and then the powder soaked is put into crucible and heated using batch-type furnace, be attached to powder surface
Cobaltous sulfate-sodium hypophosphite activating solution can occur thermal redox reaction, in tungsten carbide powder Surface Creation metallic cobalt, lived
Change powder, reaction equation is：
Co2++2H2PO2 -+2H2O→Co+2H2PO3 -+2H++H2
(4) the activation powder that step (2) obtains is subjected to plating in chemical plating fluid, filters and dry afterwards,
Obtain the tungsten-carbide powder of the uniform cobalt layers of coating surface.
Wherein, in step (1), WC granularity is 3~5 μm.
In step (1), tungsten carbide powder is added by 20~500g/L useful load and is roughened into coarsening solution, its
In, the volume ratio of hydrofluoric acid and nitric acid is 3 in hydrofluoric acid-nitric acid coarsening solution:2.Specifically, the hydrofluoric acid-nitric acid coarsening solution
In 40% fluohydric acid content be 60ml/L, 65% nitric acid content is 40ml/L.
In step (1), ultrasonic frequency is 30~40kHz, and ultrasonic power is 100~150W, a certain specific
In embodiment, ultrasonic disperse is carried out to powder using KQ3200DE types ultrasonic cleaner；60~90 DEG C of drying temperature, during drying
Between be 12~24h, in a certain specific embodiment, powder is dried using DHG-9053A Constant Temp. Ovens.
In step (2), by the tungsten carbide powder after roughening treatment by 20~200g/L useful load add to cobaltous sulfate-
Being activated in sodium hypophosphite activating solution, Cobalt monosulfate heptahydrate content is 40~50g/L in cobaltous sulfate-sodium hypophosphite activating solution,
One hydration sodium hypophosphite content is 40~50g/L.
In step (2), soak time of the roughening powder in activating solution is 30~120min.Preferably, soak time
For 60min.
Preferably, in step (2), the programming rate of batch-type furnace is 5~10 DEG C/min, heat treatment temperature is 160~
220 DEG C, soaking time is 60~120min.
In step (3), the tungsten carbide powder after activation process is added to chemical plating by 20~200g/L useful load
Being reacted in liquid, the composition of chemical plating fluid is 30~50g/L of Cobalt monosulfate heptahydrate, a hydration sodium hypophosphite content is 30~
50g/L, two citric acid monohydrate sodium contents are 50-70g/L, and boric acid content is 20~30g/L.
In step (3), chemical plating fluid phase reaction occurs system pH and controlled in 9-12, and chemical plating fluid is placed in water-bath
Heat and mechanical agitation, at 70~90 DEG C, stirring rod rotating speed be 300~500r/min for bath temperature control, plating time for 5~
15min。
In step (3), the cobalt granule particle diameter of institute's plating is 50nm~100nm.
Beneficial effect：Compared with prior art, the invention provides a kind of preparation carbonization simple to operate, repeatability is high
The method of tungsten-Co composite powder, realize that WC's and Co is dispersed by simplifying pretreatment and chemical plating, and simple to operate,
Repeatability is high, safe and reliable, saving cost.Tungsten-cobalt carbide composite prepared by the present invention can be used as alloy material, magnetic material
Material etc. is applied to the fields such as mine instrument, telecommunications, building.
Brief description of the drawings
Fig. 1 is the XRD spectrum of the powder prepared at a temperature of different drawings；Wherein, Fig. 1 (a) is the XRD of embodiment 2
Spectrum, the powder for showing to activate under the conditions of activation temperature is 220 DEG C can successfully carry out electroless cobalt plating, and Fig. 1 (b) is in embodiment 5
The tungsten-cobalt carbide powder collection of illustrative plates of acquisition, show that the powder surface in 150 DEG C of activation temperature condition activation can not successfully carry out chemistry
Cobalt plating；
Fig. 2 is the SEM surface topography maps of the powder prepared under different temperatures, wherein, used by Fig. 2 (a) is embodiment
The SEM surface topography maps of tungsten carbide original powder, powder surface are relatively smooth；It in embodiment 5 in activation temperature is 160 that Fig. 2 (b), which is,
The powder SEM surface topography maps activated under the conditions of DEG C；Fig. 2 (c) is be 220 DEG C in activation temperature in embodiment 2 under the conditions of activate
Powder SEM surface topography maps, activation it is more abundant；Fig. 2 (d) is the SEM tables of the electroless cobalt plating powder prepared in embodiment 2
Face shape appearance figure, show tungsten carbide powder surface success plating cobalt layers；
Fig. 3 is a kind of flow signal of the method for chemical plating cobalt coated tungsten carbide based on cobalt salt activation proposed by the present invention
Figure.
Embodiment
The present invention is described in detail below by specific embodiment.
Embodiment 1
Preparation method schematic flow sheet of the present invention is placed in 100ml as shown in figure 3, the WC powder 2g for taking average granularity to be 5 μm
Carry out roughening treatment in hydrofluoric acid-nitric acid mixed aqueous solution under the conditions of ultrasonic disperse, hydrofluoric acid concentration 60ml/L, nitric acid is dense
Spend for 40ml/L, coarsening time 30min.Powder filtering drying is put into cobaltous sulfate-sodium hypophosphite activating solution in ultrasonic disperse
Soaked under environment, Cobalt monosulfate heptahydrate content is 40g/L in activating solution, and a hydration sodium hypophosphite content is 40g/L, immersion
Time is 60min.Then the powder soaked is put into crucible and heated using batch-type furnace, heating rate during heating
For 10 DEG C/min, heat treatment temperature is 180 DEG C, after heating, is attached to cobaltous sulfate-sodium hypophosphite activating solution of powder surface
Thermal redox reaction can occur, tungsten carbide surface is activated.Powder after activation is put into the chemical plating fluid prepared, seven
Cobalt sulfate hydrate 50g/L, a hydration sodium hypophosphite content are 40g/L, and two citric acid monohydrate sodium contents are 70g/L, boric acid content
For 25g/L, pH value is adjusted to 9, and bath temperature is controlled at 80 DEG C, and stirring rod rotating speed is 350r/min, plating time 15min.
Powder after chemical plating is filtered and dried, obtaining coating surface has the tungsten carbide particle of uniform cobalt metal.
Embodiment 2
The WC powder 2g for taking average granularity to be 5 μm, is placed in 100ml hydrofluoric acid-nitric acid mixed aqueous solution in ultrasonic disperse
Under the conditions of carry out roughening treatment, hydrofluoric acid concentration 60ml/L, concentration of nitric acid 40ml/L, coarsening time 30min.By powder mistake
Filter drying is put into cobaltous sulfate-sodium hypophosphite activating solution is soaked under ultrasonic disperse environment, seven hydrated sulfuric acid in activating solution
Cobalt content is 50g/L, and a hydration sodium hypophosphite content is 50g/L, soak time 60min.Then the powder soaked is put
Enter in crucible and heated using batch-type furnace, heating rate is 10 DEG C/min during heating, and heat treatment temperature is 220 DEG C, is added
After heat treatment, thermal redox reaction, tungsten carbide surface can be occurred by being attached to cobaltous sulfate-sodium hypophosphite activating solution of powder surface
It is activated (activation effect is shown in Fig. 2 (c)).Powder after activation is put into the chemical plating fluid prepared, Cobalt monosulfate heptahydrate
50g/L, a hydration sodium hypophosphite content is 40g/L, and two citric acid monohydrate sodium contents are 50g/L, boric acid content 25g/L, pH
Value is adjusted to 11, and bath temperature is controlled at 80 DEG C, and stirring rod rotating speed is 350r/min, plating time 15min.By chemical plating
Powder afterwards is filtered and dried, and obtaining coating surface has the tungsten carbide particle of uniform cobalt metal.Under the conditions of 220 DEG C of heat treatment temperature
Tungsten carbide powder after activation can successfully realize surface cobalt plating, be evenly distributed.
Embodiment 3
The WC powder 2g for taking average granularity to be 5 μm, is placed in 100ml hydrofluoric acid-nitric acid mixed aqueous solution in ultrasonic disperse
Under the conditions of carry out roughening treatment, hydrofluoric acid concentration 60ml/L, concentration of nitric acid 40ml/L, coarsening time 30min.By powder mistake
Filter drying is put into cobaltous sulfate-sodium hypophosphite activating solution is soaked under ultrasonic disperse environment, seven hydrated sulfuric acid in activating solution
Cobalt content is 60g/L, and a hydration sodium hypophosphite content is 60g/L, soak time 60min.Then the powder soaked is put
Enter in crucible and heated using batch-type furnace, heating rate is 10 DEG C/min during heating, and heat treatment temperature is 200 DEG C, is added
After heat treatment, thermal redox reaction, tungsten carbide surface can be occurred by being attached to cobaltous sulfate-sodium hypophosphite activating solution of powder surface
It is activated.Powder after activation is put into the chemical plating fluid prepared, Cobalt monosulfate heptahydrate 30g/L, a hydration sodium hypophosphite
Content is 30g/L, and two citric acid monohydrate sodium contents are 50g/L, boric acid content 25g/L, and pH value is adjusted to 10, bath temperature control
For system at 80 DEG C, stirring rod rotating speed is 350r/min, plating time 15min.Powder after chemical plating is filtered and dried, is obtained
Coating surface has the tungsten carbide particle of uniform cobalt metal.
Embodiment 4
The WC powder 2g for taking average granularity to be 5 μm, is placed in 100ml hydrofluoric acid-nitric acid mixed aqueous solution in ultrasonic disperse
Under the conditions of carry out roughening treatment, hydrofluoric acid concentration 60ml/L, concentration of nitric acid 40ml/L, coarsening time 30min.By powder mistake
Filter drying is put into cobaltous sulfate-sodium hypophosphite activating solution is soaked under ultrasonic disperse environment, seven hydrated sulfuric acid in activating solution
Cobalt content is 60g/L, and a hydration sodium hypophosphite content is 60g/L, soak time 60min.Then the powder soaked is put
Enter in crucible and heated using batch-type furnace, heating rate is 10 DEG C/min during heating, and heat treatment temperature is 180 DEG C, is added
After heat treatment, thermal redox reaction, tungsten carbide surface can be occurred by being attached to cobaltous sulfate-sodium hypophosphite activating solution of powder surface
It is activated.Powder after activation is put into the chemical plating fluid prepared, Cobalt monosulfate heptahydrate 50g/L, a hydration sodium hypophosphite
Content is 40g/L, and two citric acid monohydrate sodium contents are 60g/L, boric acid content 25g/L, and pH value is adjusted to 12, bath temperature control
For system at 80 DEG C, stirring rod rotating speed is 350r/min, plating time 15min.Powder after chemical plating is filtered and dried, is obtained
Coating surface has the tungsten carbide particle of uniform cobalt metal.
Embodiment 5 (contrasts) with embodiment 2
The WC powder 2g for taking average granularity to be 5 μm, is placed in 100ml hydrofluoric acid-nitric acid mixed aqueous solution in ultrasonic disperse
Under the conditions of carry out roughening treatment, hydrofluoric acid concentration 60ml/L, concentration of nitric acid 40ml/L, coarsening time 30min.By powder mistake
Filter drying is put into cobaltous sulfate-sodium hypophosphite activating solution is soaked under ultrasonic disperse environment, seven hydrated sulfuric acid in activating solution
Cobalt content is 50g/L, and a hydration sodium hypophosphite content is 50g/L, soak time 60min.Then the powder soaked is put
Enter in crucible and heated using batch-type furnace, heating rate is 10 DEG C/min during heating, and heat treatment temperature is 160 DEG C, is added
After heat treatment, thermal redox reaction, tungsten carbide surface can be occurred by being attached to cobaltous sulfate-sodium hypophosphite activating solution of powder surface
It is activated (activation effect is shown in Fig. 2 (b)).Powder after activation is put into the chemical plating fluid prepared, Cobalt monosulfate heptahydrate
50g/L, a hydration sodium hypophosphite content is 40g/L, and two citric acid monohydrate sodium contents are 50g/L, boric acid content 25g/L, pH
Value is adjusted to 11, and bath temperature is controlled at 80 DEG C, and stirring rod rotating speed is 350r/min, plating time 15min.By chemical plating
Powder afterwards is filtered and dried, and obtains dried powder.Shown in the XRD spectrum of the powder of acquisition such as Fig. 1 (b), show be heat-treated
Tungsten carbide powder after being activated under the conditions of 150 DEG C of temperature can not realize the uniform and stable cobalt plating in surface, the heat treatment temperature of activation stage
Degree is extremely important to activation effect.
Embodiment 6 (contrasts) with embodiment 2
The WC powder 2g for taking average granularity to be 5 μm, is placed in 100ml hydrofluoric acid-nitric acid mixed aqueous solution in ultrasonic disperse
Under the conditions of carry out roughening treatment, hydrofluoric acid concentration 60ml/L, concentration of nitric acid 40ml/L, coarsening time 30min.By powder mistake
Filter drying is put into cobaltous sulfate-sodium hypophosphite activating solution is soaked under ultrasonic disperse environment, seven hydrated sulfuric acid in activating solution
Cobalt content is 50g/L, and a hydration sodium hypophosphite content is 50g/L, soak time 60min.Then the powder soaked is put
Enter in crucible and heated using batch-type furnace, heating rate is 10 DEG C/min during heating, and heat treatment temperature is 220 DEG C, is added
After heat treatment, powder is put into the chemical plating fluid prepared, Cobalt monosulfate heptahydrate 50g/L, and a hydration sodium hypophosphite content is
40g/L, two citric acid monohydrate sodium contents are 50g/L, boric acid content 25g/L, and pH value is adjusted to 11, and bath temperature control exists
50 DEG C, stirring rod rotating speed is 350r/min, retention time 15min, and chemical plating fluid can not react.Test result indicates that
Based on the electroless plating reaction carried out under this activation condition, chemical plating bath temperature is extremely important to chemical plating effect.
Claims (10)
- A kind of 1. method of the chemical plating cobalt coated tungsten carbide based on cobalt salt activation, it is characterised in that comprise the following steps：(1) tungsten carbide powder is added in hydrofluoric acid-nitric acid coarsening solution, is roughened under ultrasonic disperse effect, then filters and dry It is dry, obtain being roughened powder；(2) the roughening powder that step (1) obtains is added in cobaltous sulfate-sodium hypophosphite activating solution to enter under ultrasonic disperse environment Row immersion treatment；(3) and then the powder soaked is put into crucible and heated using batch-type furnace, be attached to the sulphur of powder surface Thermal redox reaction can occur for sour cobalt-sodium hypophosphite activating solution, in tungsten carbide powder Surface Creation metallic cobalt, obtain activating powder Body, reaction equation are：Co2++2H2PO2 -+2H2O→Co+2H2PO3 -+2H++H2(4) the activation powder that step (2) obtains is subjected to plating in chemical plating fluid, filters and dry afterwards, obtain surface plating Cover the tungsten-carbide powder of uniform cobalt layers.
- 2. preparation method according to claim 1, it is characterised in that in step (1), WC granularity is 3~5 μm.
- 3. preparation method according to claim 1, it is characterised in that in step (1), by tungsten carbide powder by 20~ 500g/L useful load adds to be roughened into coarsening solution, wherein, the body of hydrofluoric acid and nitric acid in hydrofluoric acid-nitric acid coarsening solution Product is than being 3:2.
- 4. preparation method according to claim 1, it is characterised in that in step (1), ultrasonic frequency be 30~ 40kHz, ultrasonic power are 100~150W；60~90 DEG C of drying temperature, drying time are 12~24h.
- 5. preparation method according to claim 1, it is characterised in that in step (2), by the tungsten carbide after roughening treatment Powder is added into cobaltous sulfate-sodium hypophosphite activating solution by 20~200g/L useful load and activated, cobaltous sulfate-sodium hypophosphite Cobalt monosulfate heptahydrate content is 40~50g/L in activating solution, and a hydration sodium hypophosphite content is 40~50g/L.
- 6. preparation method according to claim 1, it is characterised in that in step (2), roughening powder is in activating solution Soak time is 30~120min.
- 7. preparation method according to claim 1, it is characterised in that in step (2), the programming rate of batch-type furnace is 5 ~10 DEG C/min, heat treatment temperature is 160~220 DEG C, and soaking time is 60~120min.
- 8. preparation method according to claim 1, it is characterised in that in step (3), by the tungsten carbide after activation process Powder is added by 20~200g/L useful load to be reacted into chemical plating fluid, and the composition of chemical plating fluid is Cobalt monosulfate heptahydrate 30~50g/L, a hydration sodium hypophosphite content is 30~50g/L, and two citric acid monohydrate sodium contents are 50-70g/L, boric acid content For 20~30g/L.
- 9. preparation method according to claim 1, it is characterised in that in step (3), chemical plating fluid phase reaction generating body It is that pH value is controlled in 9-12, chemical plating fluid is placed in heating and mechanical agitation in water-bath, bath temperature is controlled at 70~90 DEG C, stirred It is 300~500r/min to mix rod rotating speed, and plating time is 5~15min.
- 10. preparation method according to claim 1, it is characterised in that in step (3), the cobalt granule particle diameter of institute's plating For 50nm~100nm.
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| CN109338197A (en) * | 2018-11-06 | 2019-02-15 | 河海大学 | A kind of preparation method of high-compactness WC/Co composite material hard alloy |
| CN111961941A (en) * | 2020-09-02 | 2020-11-20 | 四川大学 | Preparation method of superfine hard alloy cutter material |
| CN111961941B (en) * | 2020-09-02 | 2021-02-12 | 四川大学 | Preparation method of superfine hard alloy cutter material |
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Application publication date: 20180403 |