CN206721356U - A kind of workpiece with boron-richization tungsten coating - Google Patents

A kind of workpiece with boron-richization tungsten coating Download PDF

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Publication number
CN206721356U
CN206721356U CN201720311824.XU CN201720311824U CN206721356U CN 206721356 U CN206721356 U CN 206721356U CN 201720311824 U CN201720311824 U CN 201720311824U CN 206721356 U CN206721356 U CN 206721356U
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China
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tungsten
boron
richization
workpiece
coating
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CN201720311824.XU
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Chinese (zh)
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唐永炳
石磊
蒋春磊
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Shenzhen Institute of Advanced Technology of CAS
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Shenzhen Institute of Advanced Technology of CAS
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Abstract

The utility model provides a kind of workpiece with boron-richization tungsten coating, including workpiece substrate, and tungsten layer, tungsten boride gradient layer and the boron-richization tungsten coating being set in turn on the workpiece substrate;Thickness direction along from the workpiece substrate to the tungsten layer, the Boron contents in the tungsten boride gradient layer gradually increase;Crystal grain in the boron-richization tungsten coating is WBy, wherein, y is 2.5 4 numerical value.Unique coating structure in the utility model, the bond strength of each interlayer can be made by height, modulus of elasticity and thermal coefficient of expansion between each layer change in gradient from matrix to top film, and the stress of Bulk coat is down to and gone to zero, and improve the toughness and adhesion of boron-richization tungsten coating.

Description

A kind of workpiece with boron-richization tungsten coating
Technical field
Diamond coatings preparing technical field is the utility model is related to, more particularly to a kind of with boron-richization tungsten coating Workpiece.
Background technology
Transition metal boride has that fusing point is high, hardness is big, the premium properties such as wear-resisting.Can be used as cutter, mould and The coating material of other workpiece.With the continuous development of modern manufacturing industry, the requirement to machining accuracy and processing efficiency is also continuous Improve, high-speed cutting, DRY CUTTING are arisen at the historic moment, and many ordinary rigid coating materials have been difficult to meet processing request, and this is just The research to novel super-hard coating material is expedited the emergence of.And the transition metal boride (the boron-rich compound of transition metal) that Boron contents are higher Because having higher intensity, and favored by professional.However, the boron-rich compound of transition metal increases it with Boron contents Hardness height, but corresponding film substrate bond strength reduces, it is difficult to go out the good coating of adhesiveness in substrate deposit, becomes Its main bottleneck in industrial development.
Utility model content
In consideration of it, the utility model provides a kind of workpiece with boron-richization tungsten coating, it passes through on workpiece substrate A metal tungsten layer is first deposited, the increased tungsten boride transition zone of a redeposited Boron contents gradient, Boron contents is finally deposited and immobilizes Boron-richization tungsten coating, to solve the fracture toughness of boronation tungsten coating difference and the problems such as film substrate bond strength is low.
In a first aspect, this application provides a kind of workpiece with boron-richization tungsten coating, including workpiece substrate, and successively Tungsten layer, tungsten boride gradient layer and the boron-richization tungsten coating being arranged on the workpiece substrate;Along the workpiece substrate to the tungsten The thickness direction of layer, the Boron contents in the tungsten boride gradient layer gradually increase;Crystal grain in the boron-richization tungsten coating is WBy, wherein, y is 2.5-4 numerical value.
Preferably, the y is 2.5,3,3.3 or 4.Further, the y is 3 or 4.
Alternatively, the thickness of the boron-richization tungsten coating is 0.3-1.5 μm.More preferably 0.6-1.2 μm.The richness Crystallite dimension in boronation tungsten coating is 50-100 nanometers.
In the application, the crystal grain in the tungsten boride gradient layer is WBx, wherein, x span is 0~t, t is 2~ 4.Preferably 2.5~4.More preferably 3 or 4.
Alternatively, the Boron contents (molar content) in the tungsten boride gradient layer are gradually increased to 75-80% by zero.
In the application, metal tungsten layer can improve tungsten boride and be firmly bonded on matrix as prime coat, its presence;Boron Change in tungsten gradient layer, Boron contents gradually increase, its composition, hardness and the equal distribution gradient of thermal coefficient of expansion, the production without new interface The interface of raw and composition mutation;The presence of tungsten boride gradient layer, make have gradual change between boron-richization tungsten coating and metal tungsten layer The transitional link of change, effectively improves the bond strength of each interlayer, and the stress of Bulk coat is down to and gone to zero, and improves overall Toughness and adhesion.
In the application, the thickness of tungsten layer, tungsten boride gradient layer and boron-richization tungsten coating can be set according to being actually needed, such as Set according to the size of workpiece, purposes etc..
The material of the workpiece substrate can be hard alloy, stainless steel.Workpiece substrate can be cutter or other instruments (such as mould), component of machine (such as Aero-Space, automotive field).
Alternatively, the thickness of the tungsten layer is 0.1-0.3 μm.
In the application, in order that boron-richization tungsten coating obtains more preferable film substrate bond strength, the setting of boron-richization tungsten coating Thickness preferably no more than 4 times of tungsten boride gradient layers thickness, such as can be 1-3 times or 1-2 times the tungsten boride ladder Spend the thickness of layer.
Alternatively, the thickness of the tungsten boride gradient layer is 0.3-0.5 μm.The tungsten boride gradient layer of suitable depth, favorably In forming good intermediate layer, it can ensure that tungsten layer is perfectly adhered to matrix surface, and be subsequent deposition tungsten boride Gradient layer and the boron-richization tungsten coating offer good basis, and will not cause and make boron-richization tungsten coating because transition zone is blocked up The decrease of bond strength between matrix.
Further, in the tungsten boride gradient layer, WBxGrain size be Nano grade, can be specifically that 30-80 receives Rice.
The workpiece with boron-richization tungsten coating that the application first aspect provides, by being applied in workpiece substrate and rich tungsten boride Boron contents gradual increased tungsten boride gradient layer by zero is set between layer, while high rigidity is ensured so that boron-richization The fracture toughness of tungsten coating is higher, improves the adhesion between boron-richization tungsten coating and workpiece substrate.
Correspondingly, the application second aspect provides a kind of preparation method of the workpiece with boron-richization tungsten coating, including Following steps:
Workpiece substrate is provided, pre-treatment is carried out to the workpiece substrate;The pre-treatment includes ultrasonic cleaning, aura cleaning One or more in being cleaned with ion etching;
Tungsten layer is deposited on the workpiece substrate;
Using tungsten target and boron target as target, tungsten boride gradient layer is first deposited on the tungsten layer by the way of magnetron sputtering Redeposited boron-richization tungsten coating, keep the power of the tungsten target constant in deposition process, the power of the boron target is gradually increased, Keep constant afterwards, obtain the workpiece with boron-richization tungsten coating;Wherein, the crystal grain in the boron-richization tungsten coating is WBy, its In, y is 2.5-4 numerical value.
It in the embodiment of the application one, can be first cleaned by ultrasonic, the substrate after ultrasonic cleaning is placed in one afterwards In the vacuum chamber of filming equipment, aura cleaning is first carried out, then carry out ion etching cleaning.It can so better ensure that pending The cleannes of workpiece surface, to obtain the surface that more preferable deposition prepares diamond coatings.
Wherein, the ultrasonic cleaning is to carry out ultrasonic 5-30min in deionized water, acetone, ethanol successively.Ultrasonic clear , it is necessary to which substrate is dried up after washing, then carry out other pretreatments.
The aura cleaning and ion etching cleaning are carried out in the vacuum chamber of a filming equipment;Aura cleaning and It is 5.0 × 10 that the ion etching cleaning, which is required in vacuum,-3Below Pa carry out.
Specifically, the condition of the aura cleaning is:It is passed through argon gas into vacuum chamber, 300~500sccm of argon flow amount, Operating air pressure is 1.0~1.7Pa, and the back bias voltage loaded on matrix frame is -500~-800V, and the time of aura cleaning is 10~30min.
Specifically, the condition of the ion etching cleaning is:Open ion gun, argon gas is passed through into vacuum chamber, control from The voltage of component is 50~90V, and argon flow amount is 70~500sccm, and intracavitary air pressure is 0.5~1.2Pa, and matrix loading biases For -100~-800V;The time of the ion etching cleaning is 10~30min.
In the embodiment of the application one, the depositional mode of the tungsten layer is magnetron sputtering method, is specifically included:Target is made with tungsten Material, the power for applying tungsten target material are 1-2.4kW, and sputtering atmosphere is ar gas environment, and intracavitary pressure during sputtering is 0.2-1.3Pa, Cavity temperature is 350~600 DEG C, and matrix frame is biased at -100~-300V.Alternatively, sedimentation time is 2~10min.This The depositional mode that sputtering is not limited in application prepares tungsten layer.
In the application, during the redeposited boron-richization tungsten coating of the first deposition tungsten boride gradient layer, in control chamber Pressure is 0.4-1.0Pa, and 350~500 DEG C of depositing temperature, matrix frame is biased at -30~-200V;Keep the power of tungsten target For 300~500W, the power of the boron target is gradually increased to 1-2.4kW from zero.
Alternatively, the power increase rate of the boron target is 1~10W/s.Alternatively, kept not in the power of the boron target After change, 40~100min of redeposition.
Alternatively, the thickness of the tungsten boride gradient layer is 0.3-0.5 μm.
Alternatively, the thickness of the boron-richization tungsten coating is 0.3-1.5 μm.More preferably 0.6-1.2 μm.
The preparation method for the workpiece with boron-richization tungsten coating that the application provides, by the complete metal tungsten layer of matrix deposition Afterwards, the increased tungsten boride gradient layer of Boron contents is first deposited, the constant boron-richization tungsten coating of redeposited Boron contents, can be effectively improved The bond strength of each interlayer, the modulus of elasticity between each layer and thermal coefficient of expansion is set to change in gradient from matrix to top film, The stress of Bulk coat is down to and gone to zero, improves the toughness and adhesion of boron-richization tungsten coating.The application is heavy using same Product equipment, you can realize tungsten layer, tungsten boride gradient layer, the continuity of boron-richization tungsten coating and prepare, whole process time Greatly shorten, technological parameter is easily controllable, prepares cost and is greatly reduced, is highly suitable for large-scale industrial production.
The advantages of the application, will partly illustrate in the following description, and a part is apparent according to specification , or can be known by the implementation of the embodiment of the present application.
Brief description of the drawings
Fig. 1 is the structural representation of the workpiece in the utility model embodiment with boron-richization tungsten coating.
Embodiment
As described below is the preferred embodiment of the embodiment of the present application, it is noted that for the common skill of the art For art personnel, on the premise of the embodiment of the present application principle is not departed from, some improvements and modifications can also be made, these improvement The protection domain of the embodiment of the present application is also considered as with retouching.
Embodiment 1
A kind of preparation method of the workpiece with boron-richization tungsten coating, comprises the following steps:
(1) substrate pretreated:
YG6X (WC-6wt.%Co) the hard alloy transposition blades sold using on domestic market are as matrix, first with steaming The matrix is cleaned by ultrasonic 10min by distilled water, then is cleaned by ultrasonic 20min with acetone and absolute ethyl alcohol successively, then with nitrogen by base Body dries up, and is put into air dry oven in 80-100 DEG C of drying;
Above-mentioned matrix after drying is fixed on ion gun/arc ion plating composite coating equipment (producer:Tie up titanium in Dalian Gram, MF610/610 models) on pivoted frame in vacuum chamber;Door for vacuum chamber is closed, opens water cooling unit by ion gun, multiple arc target, molecule Pump, the water route of vacuum chamber are connected, and open the general supply of air compressor machine and composite film coating machine, be then turned on mechanical pump and side take out valve with And molecular pump, molecular pump is entered climb mode;After molecular pump reaches full speed, close side and take out valve, roughing valve is opened, to true Empty room is slightly taken out;After vacuum chamber internal pressure reaches below 10Pa by force, it is again turned on side and takes out valve;When pressure in vacuum tank reaches 3Pa After below, roughing valve is closed, opens high threshold to vacuum chamber pumping high vacuum.When pressure in vacuum tank is extracted into 5.0 × 10-3After Pa, beat Open heating power supply and heated baking is carried out to vacuum chamber, heating-up temperature is 350 DEG C, and turret system is opened in heating process, makes sample Public autobiography is carried out, matrix frame rotating speed is 20 revs/min;When vacuum reaches 3.0 × 10-3During Pa, aura cleaning is proceeded by;
After aura cleaning terminates, open ion gun and icon bombardment cleaning, ion source voltage 90V, argon gas are carried out to sample Flow 200sccm, the operating air pressure of argon gas is 1.0Pa, and the bias of matrix loading is -200V;Ion gun scavenging period is 30min;
(2) deposition of metal tungsten layer:After above-mentioned ion etching cleaning terminates, argon gas is passed through into vacuum chamber, adjusts argon Throughput makes the pressure of vacuum chamber be 1.3Pa, opening metal tungsten target, and the power for controlling W targets is 2.4KW, substrate bias for- 100V, sedimentation time 3min;The thickness of gained tungsten layer is 0.1 μm.
(3) after metal tungsten layer deposition terminates, argon gas is passed through into vacuum chamber, regulation mass flowmenter makes the pressure in vacuum chamber Strong is 0.8Pa, and substrate bias is -150V, and using tungsten target and boron target as target, it is 600W to keep metal W target power output, by B targets Power is started from scratch is gradually increased to 2.4kW with 1W/s speed, obtains Boron contents gradually increased tungsten boride gradient layer;
The power for keeping B targets afterwards is that 2.4kW and W target power outputs are 600W, continues to deposit 100min, obtains rich tungsten boride and applies Layer;
(4) after coating deposition terminates, ion source current and grid bias power supply are closed, be then shut off gas mass flow gauge and Gas cylinder main valve and pressure-reducing valve;Cooling process is set, after temperature is dropped to below 100 DEG C, high threshold is closed, opens vent valve, is treated true When pressure is consistent with ambient pressure in empty room, door for vacuum chamber is opened, then takes out sample.
Fig. 1 is the structural representation of the workpiece with boron-richization tungsten coating prepared by the utility model embodiment 1;In figure, 101 be workpiece substrate, and 102 be tungsten layer, and 103 be Boron contents gradually increased tungsten boride gradient layer, and 104 be boron-richization tungsten coating.
In the present embodiment, the thickness of gained tungsten boride gradient layer 103 is 0.5 μm, along the workpiece substrate to the tungsten layer Thickness direction, B content is gradually increased to 80% by zero in tungsten boride gradient layer;The thickness of boron-richization tungsten coating 104 For 1.2 μm, crystallite dimension is 80nm or so, crystal grain WB4
Embodiment 2
A kind of preparation method of the workpiece with boron-richization tungsten coating, comprises the following steps:
(1) substrate pretreated:
YG8 (WC-8%Co) the hard alloy transposition blades sold using on domestic market use distilled water first as matrix The matrix is cleaned by ultrasonic 5min, then is placed in acetone and is cleaned by ultrasonic 15 minutes, places into absolute ethyl alcohol be cleaned by ultrasonic afterwards 10min, then matrix is dried up with nitrogen, and be put into 100 DEG C of drying in air dry oven;
Above-mentioned matrix after drying is fixed in the vacuum chamber of ion gun/arc ion plating composite coating equipment, adopted 3.0 × 10 are evacuated to mode same as Example 1-3Pa, open argon bottle main valve, pressure-reducing valve, ion gun valve, arc valve and target valve And mass flowmenter is passed through argon gas into vacuum chamber and carries out aura cleaning to matrix, wherein, the condition of aura cleaning is to true It is passed through argon gas in empty room, argon flow amount 400sccm, operating pressure 1.4Pa, substrate bias -500V, aura scavenging period is 30min;
After aura cleaning terminates, open ion gun and icon bombardment cleaning is carried out to sample, Ion Cleaning condition is:Ion gun Voltage is 50V, and argon flow amount 70sccm, the operating air pressure of argon gas is 0.5Pa, and substrate bias is -100V, and matrix frame rotating speed is 20 Rev/min;Ion gun scavenging period is 30min;
(2) deposition of metal tungsten layer:After above-mentioned Ion Cleaning terminates, argon gas is passed through into vacuum chamber, adjusts argon gas stream Amount makes the pressure of vacuum chamber be 1.0Pa, and opening metal tungsten target, the power for controlling W targets is 2KW, and substrate bias is -150V, deposition Time is 7min;The thickness of gained tungsten layer is 0.2 μm.
(3) after metal tungsten layer deposition terminates, argon gas is passed through into vacuum chamber, regulation mass flowmenter makes the pressure in vacuum chamber Strong is 0.9Pa, and substrate bias is -80V, and depositing temperature is 400 DEG C, using tungsten target and boron target as target, keeps metal W target power output For 500W, the power of B targets is started from scratch 2.0kW is gradually increased to 10W/s speed, obtain Boron contents gradually increased boron Change tungsten gradient layer;
The power for keeping B targets afterwards is that 2.0kW and W target power outputs are 500W, continues to deposit 100min, obtains rich tungsten boride and applies Layer;
(4) after coating deposition terminates, ion source current and grid bias power supply are closed, be then shut off gas mass flow gauge and Gas cylinder main valve and pressure-reducing valve;Cooling process is set, after temperature is dropped to below 100 DEG C, high threshold is closed, opens vent valve, is treated true When pressure is consistent with ambient pressure in empty room, door for vacuum chamber is opened, then takes out sample.
In the present embodiment, the thickness of gained tungsten boride gradient layer is 0.3 μm, the thickness along the workpiece substrate to the tungsten layer Direction is spent, B content is gradually increased to 80% by zero in tungsten boride gradient layer;The thickness of boron-richization tungsten coating is 0.9 μm, Crystallite dimension is 90 rans, crystal grain WB4
Embodiment 3
A kind of preparation method of the workpiece with boron-richization tungsten coating, comprises the following steps:
(1) substrate pretreated:
YT15 (WC-15%TiC) the hard alloy transposition blades sold using on domestic market are as matrix, first with distillation The matrix is cleaned by ultrasonic 20min by water, then is placed in acetone and is cleaned by ultrasonic 10 minutes, and it is clear to place into ultrasound in absolute ethyl alcohol afterwards 15min is washed, is then dried up matrix with nitrogen, and is put into 120 DEG C of drying in air dry oven;
Above-mentioned matrix after drying is fixed in the vacuum chamber of ion gun/arc ion plating composite coating equipment, adopted 2.0 × 10 are evacuated to mode same as Example 1-3Pa, open argon bottle main valve, pressure-reducing valve, ion gun valve, arc valve and target valve And mass flowmenter is passed through argon gas into vacuum chamber and carries out aura cleaning to matrix, wherein, the condition of aura cleaning is to true Argon gas is passed through in empty room, argon flow amount 500sccm, operating pressure 1.5Pa, substrate bias -600V, it is clear that aura is carried out to substrate Wash 20min;
After aura cleaning terminates, open ion gun and icon bombardment cleaning is carried out to sample, ion etching cleaning condition is:From Component voltage is 70V, and argon flow amount 150sccm, the operating air pressure of argon gas is 0.9Pa, and substrate bias is -550V;Matrix frame turns Speed is 20 revs/min, Ion Cleaning time 20min;
(2) deposition of metal tungsten layer:After above-mentioned Ion Cleaning terminates, argon gas is passed through into vacuum chamber, adjusts argon gas stream Amount makes the pressure of vacuum chamber be 0.7Pa, and opening metal tungsten target, the power for controlling W targets is 2KW, and substrate bias is -200V, deposition Time is 10min;The thickness of gained tungsten layer is 0.3 μm.
(3) after metal tungsten layer deposition terminates, argon gas is passed through into vacuum chamber, regulation mass flowmenter makes the pressure in vacuum chamber Strong is 0.4Pa, and substrate bias is -200V, and depositing temperature is 500 DEG C;Using tungsten target and boron target as target, metal W target work(is kept Rate is 300W, and the power of B targets is started from scratch and is gradually increased to 1.0kW with 5W/s speed, it is gradually increased to obtain Boron contents Tungsten boride gradient layer;
The power for keeping B targets afterwards is that 1.0kW and W target power outputs are 300W, continues to deposit 40min, obtains rich tungsten boride and applies Layer;
(4) after coating deposition terminates, ion source current and grid bias power supply are closed, be then shut off gas mass flow gauge and Gas cylinder main valve and pressure-reducing valve;Cooling process is set, after temperature is dropped to below 100 DEG C, high threshold is closed, opens vent valve, is treated true When pressure is consistent with ambient pressure in empty room, door for vacuum chamber is opened, then takes out sample.
In the present embodiment, the thickness of gained tungsten boride gradient layer is 0.4 μm, the thickness along the workpiece substrate to the tungsten layer Direction is spent, B content is gradually increased to 75% by zero in tungsten boride gradient layer;The thickness of boron-richization tungsten coating is 0.6 μm, Crystallite dimension is 50 rans, crystal grain WB3
It should be noted that according to the above description the announcement of book and with illustrate, the application those skilled in the art also Above-mentioned embodiment can be changed and changed.Therefore, the application is not limited to disclosed and described above specific real Mode is applied, some equivalent modifications and change to the application should also be as within the protection domain of claims hereof.This Outside, although having used some specific terms in this specification, these terms merely for convenience of description, not to the application Form any restrictions.

Claims (8)

1. a kind of workpiece with boron-richization tungsten coating, it is characterised in that including workpiece substrate, and be set in turn in the work Tungsten layer, tungsten boride gradient layer and boron-richization tungsten coating on part matrix;Thickness direction along from the workpiece substrate to the tungsten layer, Boron contents in the tungsten boride gradient layer gradually increase;Crystal grain in the boron-richization tungsten coating is WBy, wherein, y 2.5- 4 numerical value.
2. there is the workpiece of boron-richization tungsten coating as claimed in claim 1, it is characterised in that the thickness of the tungsten layer is 0.1- 0.3μm。
3. there is the workpiece of boron-richization tungsten coating as claimed in claim 1, it is characterised in that the thickness of the boron-richization tungsten coating 4 times of degree no more than the thickness of the tungsten boride gradient layer.
4. there is the workpiece of boron-richization tungsten coating as claimed in claim 1, it is characterised in that the thickness of the tungsten boride gradient layer Spend for 0.3-0.5 μm.
5. there is the workpiece of boron-richization tungsten coating as claimed in claim 1, it is characterised in that the thickness of the boron-richization tungsten coating Spend for 0.3-1.5 μm.
6. there is the workpiece of boron-richization tungsten coating as claimed in claim 1, it is characterised in that in the boron-richization tungsten coating Crystallite dimension is 50-100 nanometers.
7. there is the workpiece of boron-richization tungsten coating as claimed in claim 1, it is characterised in that the workpiece substrate closes for hard Gold or stainless steel.
8. there is the workpiece of boron-richization tungsten coating as claimed in claim 1, it is characterised in that the y is 2.5,3,3.3 or 4.
CN201720311824.XU 2017-03-28 2017-03-28 A kind of workpiece with boron-richization tungsten coating Withdrawn - After Issue CN206721356U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108660424A (en) * 2017-03-28 2018-10-16 深圳先进技术研究院 A kind of workpiece and preparation method thereof with boron-richization tungsten coating

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108660424A (en) * 2017-03-28 2018-10-16 深圳先进技术研究院 A kind of workpiece and preparation method thereof with boron-richization tungsten coating
CN108660424B (en) * 2017-03-28 2023-12-19 深圳先进技术研究院 Workpiece with tungsten boride-rich coating and preparation method thereof

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