CN107130227B - A kind of superfine nano-crystalline tungsten carbide coating and preparation method thereof - Google Patents

A kind of superfine nano-crystalline tungsten carbide coating and preparation method thereof Download PDF

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CN107130227B
CN107130227B CN201710545169.9A CN201710545169A CN107130227B CN 107130227 B CN107130227 B CN 107130227B CN 201710545169 A CN201710545169 A CN 201710545169A CN 107130227 B CN107130227 B CN 107130227B
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hydrogen
coating
tungsten carbide
matrix
tungsten
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CN107130227A (en
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谭成文
张慧聪
于晓东
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Haipu precision materials (Suzhou) Co.,Ltd.
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Beijing Institute of Technology BIT
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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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/32—Carbides
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • C23C16/0281—Deposition of sub-layers, e.g. to promote the adhesion of the main coating of metallic sub-layers

Abstract

The present invention relates to a kind of superfine nano-crystalline tungsten carbide coatings and preparation method thereof, for a kind of superfine nano-crystalline tungsten carbide coating prepared by the method using aumospheric pressure cvd, prepared superfine nano-crystalline tungsten carbide coating is to be especially in the presence of the W that partial size is 3~5nm with high rigidity, wear-resistant, corrosion resistance characteristic fine grain stratiform tungsten carbide coating2C superfine nano-crystalline and amorphous, effectively increase the inter-layer bonding force and coating hardness of layer structure coating, and the microhardness of the coating can achieve 28.8GPa.

Description

A kind of superfine nano-crystalline tungsten carbide coating and preparation method thereof
Technical field
The present invention relates to a kind of superfine nano-crystalline tungsten carbide coatings and preparation method thereof, use atmospheric chemical vapor to be a kind of The superfine nano-crystalline tungsten carbide coating of the method preparation of deposition, prepared superfine nano-crystalline tungsten carbide coating are with high hard Degree, wear-resistant, corrosion resistance characteristic fine grain stratiform tungsten carbide coating are especially in the presence of the W that partial size is 3~5nm2C is ultra-fine to be received Meter Jing and amorphous, effectively increase the inter-layer bonding force of layer structure coating, while improving coating hardness.
Background technique
With scientific research and industrial application deeply and development, coating abrasion and corrosion phenomenon under extreme environment It is more obvious, huge economic loss can be all caused every year.Surface Engineering is to solve the problems, such as that such important means, technique include Thermal spraying, supersonic flame spraying, physical vapour deposition (PVD) etc., chemical vapour deposition technique therein can be in inner surfaces and complex shape Preparation binding force is strong on shape matrix, coefficient of friction is low, uniform coating.Tungsten carbide has the property such as hardness is high, corrosion-resistant, wear-resistant Can, it can be used as the protective coating of equipment component under the conditions of abrasion, corrosion etc. are exceedingly odious, alleviate matrix failure, extension makes Use the service life.
Chemical vapor carbon deposition tungsten coating carries out under environment under low pressure mostly, because of molecule mean free path when low pressure Greatly, gained coating is more uniform.But low-pressure chemical vapor deposition process is complicated, equipment performance requirement is very high, and deposition rate It is relatively slow, difficulty is brought to industrial application.
Aumospheric pressure cvd simple process, it is lower to equipment requirement, and the growth rate of coating is very fast, applies when grasping After the influence factor and controlling mechanism of layer growth, can be quick by adjusting parameters such as partial pressure, overall flow rate and depositing temperatures To uniform, fine and close coating.
There are two kinds of microstructures of column crystal and stratiform fine grain, columns for the tungsten carbide coating prepared using chemical vapor deposition Brilliant tungsten carbide hardness is generally 2000 to 2500kg/mm3Though having good wear-resisting property, adjacent column crystalline substance is intercrystalline Interstitial area binding force is weaker, and there are cracking is easy when corrosive agent or corrosive media, corrosion resistance is poor；The carbonization of stratiform fine grain Tungsten coating hardness is 2400 to 3000kg/mm3, good sherardizing steel performance is shown in high and low-angle impacts, but It is that easily there is a phenomenon where crackings, delamination after coating internal stress causes its thickness to reach to a certain degree, it is difficult to it is preferable to obtain quality Thick coating.
Summary of the invention
The purpose of the invention is to overcome the deficiencies in the prior art, propose a kind of superfine nano-crystalline tungsten carbide coating and its Preparation method.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of superfine nano-crystalline tungsten carbide coating, the coating include stratiform aplitic texture and through fibrous group of multilayer It knits, exists simultaneously W and W in stratiform aplitic texture2C crystal grain, there is only W in the bacillar structure of multilayer2C crystal grain, partial size For 3~5nm, amorphous is existed simultaneously.Presence through the bacillar structure of multilayer improves the Coating combination of stratiform aplitic texture The microhardness of power and hardness, the coating can achieve 28.8GPa.
A kind of the step of preparation method of superfine nano-crystalline tungsten carbide coating, this method includes:
(1) matrix is placed in chemical vapor deposition reaction chamber, is passed through inert gas with evacuation of air, then passes to hydrogen Gas simultaneously closes inert gas；
(2) it opens heating device and matrix is heated to 550-600 DEG C, be passed through tungsten hexafluoride and make it in advance and hydrogen Mixing, tungsten hexafluoride and hydrogen occur reduction reaction and form internal layer tungsten coating on matrix；
(3) it is subsequently passed carbonaceous gas, is chemically reacted between carbonaceous gas, hydrogen and tungsten hexafluoride three, is kept Carbonaceous gas and tungsten hexafluoride are closed after setting time；
(4) it keeps supply to the matrix of hydrogen to be cooled to 50 DEG C and closes hydrogen hereinafter, opening inert gas, after emptying hydrogen Sample is taken out, the superfine nano-crystalline tungsten carbide coating for being previously deposited tungsten coating on matrix is obtained.
Inert gas in the step (1) is argon gas or nitrogen；
In the step (2), the molar ratio of tungsten hexafluoride and hydrogen is 1:2-4, preferably 1:3；
In the step (3), carbonaceous gas is dimethyl ether, and tungsten hexafluoride and dimethyl ether molar ratio are 1.6~2.9:1, Setting time is related with the deposition thickness of superfine nano-crystalline tungsten carbide coating, i.e., the longer obtained coating layer thickness of setting time is more It is thick.
Beneficial effect
It (1) can be in depositing silicon tungsten coating on the matrix of inner surface and complicated shape using the method for chemical vapor deposition；
(2) requirement and process complexity tested to equipment can be reduced using aumospheric pressure cvd, and reality is effectively reduced Test cost；
(3) it is previously deposited the binding force that tungsten coating is conducive to improve tungsten carbide coating and matrix；
(4) it deposits to have obtained the tungsten carbide coating of stratiform fine grain as carbon source using dimethyl ether, can avoid column crystal intergranular The problem of cracking, corrosion resistance reduce；
(5) use lower tungsten hexafluoride/dimethyl ether ratio that can deposit the Ultra-fine Grained W for obtaining partial size as 3~5nm2C crystal grain And amorphous, the inter-layer bonding force of coating is effectively increased, solving internal stress in stratiform aplitic texture leads to coating cracking, takes off The problem of layer.
Detailed description of the invention
Fig. 1 is the XRD diagram of tungsten carbide coating prepared by embodiment 1；
Fig. 2 includes that there is the section SEM of the tungsten carbide coating of tungsten internal layer to scheme for the preparation of embodiment 1；
Fig. 3 is the section SEM figure of tungsten carbide coating prepared by embodiment 1；
Fig. 4 is the SAD figure of tungsten carbide coating prepared by embodiment 1；
Fig. 5 is the HRTEM figure of tungsten carbide coating prepared by embodiment 1；
Specific embodiment
Below by example, the invention will be further described, but embodiment is not intended to limit protection scope of the present invention.
Embodiment 1
Copper substrate is placed in chemical vapor deposition reaction chamber, be passed through hydrogen after being passed through argon gas 10min and closes argon gas, It opens heating device and Copper substrate is heated to 600 DEG C, then pass to tungsten hexafluoride, gas of dimethyl ether, 2h are passed through after 10min Dimethyl ether and tungsten hexafluoride are closed afterwards, and the supply of hydrogen to Copper substrate is kept to be cooled to 50 DEG C hereinafter, opening argon gas and closing hydrogen Gas takes out sample after 10min.
Wherein argon flow be 2L/min, hydrogen flowing quantity 1.1L/min, WF6Flow is 5g/min, dimethyl ether flow is 200ml/min。
XRD test is carried out to obtained sample, as shown in Figure 1, as shown in Figure 1, being previously deposited the Copper substrate of tungsten coating On exist simultaneously W and W in the coating that is deposited2C；
SEM test has been carried out to obtained sample, as shown in Figures 2 and 3, as shown in Figure 2, the tungsten that Copper substrate is previously deposited Layer is columnar crystal structure, from the figure 3, it may be seen that the coating deposited on tungsten layer has layer structure and bacillar structure, and threadiness Tissue runs through multilayer laminar aplitic texture；
Selected diffraction is carried out to the bacillar structure in obtained sample coatings, as shown in figure 4, as shown in Figure 4, this spreads out Penetrating ring is polycrystalline diffraction ring, and all diffraction rings correspond to crystal face and belong to hexagonal structure W2C crystal corresponds to crystal face successively from inside to outside For (0002),
Bacillar structure in obtained sample coatings is observed using high resolution transmission electron microscopy, is obtained The high resolution transmission electron microscopy of bacillar structure in coating, as shown in figure 4, as shown in Figure 4, grain size is 3~ 5nm additionally, there may be amorphous, this is corresponding with the diffraction peaks broadening phenomenon in XRD diagram, can be with by the measurement to lattice fringe Determine that crystal grain is W2C crystal illustrates that bacillar structure is the W for being 3~5nm by partial size2C nano crystal grain and amorphous composition；
Using nano-hardness tester and continuous stiffness measurement is used to measure the microhardness of coating as 28.8GPa.
Embodiment 2
Copper substrate is placed in chemical vapor deposition reaction chamber, be passed through hydrogen after being passed through argon gas 10min and closes argon gas, It opens heating device and matrix is heated to 600 DEG C, be passed through tungsten hexafluoride, gas of dimethyl ether is passed through after 10min, is closed after 1h Dimethyl ether and tungsten hexafluoride keep the supply of hydrogen to matrix to be cooled to 50 DEG C hereinafter, open argon gas and close hydrogen, 10min After take out sample, wherein argon flow be 2L/min, hydrogen flowing quantity 1.1L/min, WF6Flow is 5g/min, dimethyl ether flow For 150ml/min.
Embodiment 3
Copper substrate is placed in chemical vapor deposition reaction chamber, be passed through hydrogen after being passed through argon gas 10min and closes argon gas, It opens heating device and matrix is heated to 550 DEG C, be passed through tungsten hexafluoride, gas of dimethyl ether is passed through after 10min, is closed after 1h Dimethyl ether and tungsten hexafluoride keep the supply of hydrogen to matrix to be cooled to 50 DEG C hereinafter, open argon gas and close hydrogen, 10min After take out sample, wherein argon flow be 2L/min, hydrogen flowing quantity 1.1L/min, WF6Flow is 5g/min, dimethyl ether flow For 150ml/min.
Embodiment 4
Copper substrate is placed in chemical vapor deposition reaction chamber, be passed through hydrogen after being passed through argon gas 10min and closes argon gas, It opens heating device and matrix is heated to 600 DEG C, be passed through tungsten hexafluoride, gas of dimethyl ether is passed through after 10min, is closed after 1h Dimethyl ether and tungsten hexafluoride keep the supply of hydrogen to matrix to be cooled to 50 DEG C hereinafter, open argon gas and close hydrogen, 10min After take out sample, wherein argon flow be 2L/min, hydrogen flowing quantity 1.1L/min, WF6Flow is 5g/min, dimethyl ether flow For 175ml/min.
Embodiment 5
Copper substrate is placed in chemical vapor deposition reaction chamber, be passed through hydrogen after being passed through argon gas 10min and closes argon gas, It opens heating device and matrix is heated to 600 DEG C, be passed through tungsten hexafluoride, gas of dimethyl ether is passed through after 10min, is closed after 1h Dimethyl ether and tungsten hexafluoride keep the supply of hydrogen to matrix to be cooled to 50 DEG C hereinafter, open argon gas and close hydrogen, 10min After take out sample, wherein argon flow be 2L/min, hydrogen flowing quantity 1.1L/min, WF6Flow is 5g/min, dimethyl ether flow For 225ml/min.

Claims (5)

1. a kind of superfine nano-crystalline tungsten carbide coating, it is characterised in that: the coating includes stratiform aplitic texture and through multilayer Bacillar structure exists simultaneously W and W in stratiform aplitic texture2C crystal grain, there are W in the bacillar structure of multilayer2C crystal grain And amorphous, W2C size of microcrystal is 3~5nm；
The step of preparation method of the superfine nano-crystalline tungsten carbide coating are as follows:
(1) matrix is placed in chemical vapor deposition reaction chamber, is passed through inert gas with evacuation of air, then passes to hydrogen simultaneously Close inert gas；
(2) it opens heating device and matrix is heated to 550-600 DEG C, be passed through tungsten hexafluoride and keep it mixed with hydrogen in advance It closes, forms internal layer tungsten coating on matrix；
(3) it is subsequently passed carbonaceous gas, the molar ratio of tungsten hexafluoride and carbonaceous gas is 1.6~2.9:1, after keeping setting time Close carbonaceous gas and tungsten hexafluoride；
(4) it keeps supply to the matrix of hydrogen to be cooled to 50 DEG C and closes hydrogen hereinafter, opening inert gas, taken out after emptying hydrogen Sample obtains product；
The molar ratio of the tungsten hexafluoride and hydrogen is 1:2-4；Carbonaceous gas is dimethyl ether.
2. a kind of preparation method of superfine nano-crystalline tungsten carbide coating, it is characterised in that the step of this method includes:
(1) matrix is placed in chemical vapor deposition reaction chamber, is passed through inert gas with evacuation of air, then passes to hydrogen simultaneously Close inert gas；
(2) it opens heating device and matrix is heated to 550-600 DEG C, be passed through tungsten hexafluoride and keep it mixed with hydrogen in advance It closes, forms internal layer tungsten coating on matrix；
(3) it is subsequently passed carbonaceous gas, the molar ratio of tungsten hexafluoride and carbonaceous gas is 1.6~2.9:1, after keeping setting time Close carbonaceous gas and tungsten hexafluoride；
(4) it keeps supply to the matrix of hydrogen to be cooled to 50 DEG C and closes hydrogen hereinafter, opening inert gas, taken out after emptying hydrogen Sample obtains product；
The molar ratio of the tungsten hexafluoride and hydrogen is 1:2-4；Carbonaceous gas is dimethyl ether.
3. a kind of superfine nano-crystalline tungsten carbide coating according to claim 1, it is characterised in that: in the step (1) Inert gas be argon gas or nitrogen.
4. a kind of superfine nano-crystalline tungsten carbide coating according to claim 1, it is characterised in that: tungsten hexafluoride and hydrogen Molar ratio is 1:3.
5. a kind of superfine nano-crystalline tungsten carbide coating according to claim 1, it is characterised in that: in the step (3), Setting time is related with the deposition thickness of superfine nano-crystalline tungsten carbide coating, i.e., the longer obtained coating layer thickness of setting time is more It is thick.
CN201710545169.9A 2017-07-06 2017-07-06 A kind of superfine nano-crystalline tungsten carbide coating and preparation method thereof Active CN107130227B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0305917A2 (en) * 1987-09-03 1989-03-08 Air Products And Chemicals, Inc. High hardness fine grained tungsten-carbon alloys and process for making same
JPH04254585A (en) * 1991-02-04 1992-09-09 Central Glass Co Ltd Formation of tungsten carbide film
CN1342215A (en) * 1999-02-11 2002-03-27 哈迪德有限公司 Tungsten carbide coatings and method for producing the same
CN101061254A (en) * 2004-10-12 2007-10-24 哈达德涂料有限公司 Alloyed tungsten produced by chemical vapour deposition
CN102242347A (en) * 2011-06-29 2011-11-16 北京理工大学 Method for preparing tungsten tube for heating body

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0305917A2 (en) * 1987-09-03 1989-03-08 Air Products And Chemicals, Inc. High hardness fine grained tungsten-carbon alloys and process for making same
JPH04254585A (en) * 1991-02-04 1992-09-09 Central Glass Co Ltd Formation of tungsten carbide film
CN1342215A (en) * 1999-02-11 2002-03-27 哈迪德有限公司 Tungsten carbide coatings and method for producing the same
CN101061254A (en) * 2004-10-12 2007-10-24 哈达德涂料有限公司 Alloyed tungsten produced by chemical vapour deposition
CN102242347A (en) * 2011-06-29 2011-11-16 北京理工大学 Method for preparing tungsten tube for heating body

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