CN109778176A - A kind of preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating - Google Patents
A kind of preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating Download PDFInfo
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- CN109778176A CN109778176A CN201910026401.7A CN201910026401A CN109778176A CN 109778176 A CN109778176 A CN 109778176A CN 201910026401 A CN201910026401 A CN 201910026401A CN 109778176 A CN109778176 A CN 109778176A
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Abstract
The invention discloses a kind of preparation methods of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating, are related to material surface engineering field.The characteristics of this method, is: firstly, suppressing prefabricated blank in proportion to titanium valve, aluminium powder;Then, with sand paper polishing matrix surface;TiAl intermetallic compound coating is obtained finally, being preheated with high-frequency induction auxiliary self-spreading method by matrix and coating and lighting self-propagating reaction.Present invention process is simple, heating efficiency is high, at low cost, and acquisition coating is smooth, fine and close, the porosity is low, bond strength is high.The surface treatment such as tool and mould and structural elements can be widely used in and remanufactured, their service life is improved.
Description
Technical field
The present invention relates to material surface engineering fields, and in particular between a kind of high-frequency induction auxiliary self-spreading TiAl system metal
The preparation method of compound coat.
Background technique
TiAl series intermetallic compound has specific gravity small, and specific stiffness and specific strength are high, and elevated temperature strength is good, uses temperature height etc.
Advantage also has many advantages, such as preferable resistant to high temperatures, anticorrosive, creep resistant and anti-fatigue performance, and focus on the application is in aerospace
Field and automotive field, such as engine blade, turbine, exhaust valve component, TiAl series intermetallic compound are considered great
One of novel light high-temperature structural material of application prospect.In order to improve the high-temperature behavior of steel, one usually is coated on its surface
Layer TiAl system metal compound coatings.In the surface engineering technology for preparing TiAl system metal compound coatings, self propagating high temperature
Synthesis (SHS) technology is a kind of quick, simple, economic and interface cleanness in-situ preparation TiAl series intermetallic compound coating
Technology.But it is faced especially when preparing shallow layer only with single SHS method preparation TiAl series intermetallic compound coating
SHS conversion zone is thin, and total thermal discharge is few, adds the good thermal conductivity of metallic matrix, and base metal surface can not be made to be in melting
State causes the binding performance of coating and metallic matrix bad.So being often required to use auxiliary thermal source by substrate preheating or promotion
The temperature of matrix surface.Compared with supersonic speed, laser, heating furnace and plasma etc., high-frequency induction has simple process, heating speed
The advantages that degree is fast, heat waste is few, heating efficiency is high, pollution-free, processing quality is high, at low cost, can be used as self- propagating composite coating
Auxiliary thermal source.But currently, using high-frequency induction auxiliary self-spreading preparation TiAl system metal compound coatings almost without.
Publication No. CN105331973A discloses a kind of titanium alloy surface and prepares high Nb titanium aluminium base alloy antioxidant coating
Method.Using the technique of laser melting coating, the laser melting coating Ti-Al-Nb mixed-powder on titanium alloy sheet then carries out vacuum to this method
(> 1150 DEG C) of high temperature are heat-treated and then obtain Ti3Al+TiAl two-phase coating.This method is that Ti and Al is anti-when reducing laser melting coating
The seasonable defect for sputtering and then causing more than coating hole and crackle is using vacuum high-temperature heat treatment, this method complex process and equipment
Valuableness should not use steel matrix.Publication No. CN103628014A discloses a kind of cavitation erosion resistant surface Ti-Al treated coating of titanium alloy
Preparation method.This method obtains the diffusion annealing for carrying out 550-1000 DEG C after titanium alloy elder generation dip calorizing in argon gas or vacuum again
TiAl3Coating, this method are not suitable for steel matrix.Publication No. CN103898465A discloses titanium alloy surface magnetron sputtering and prepares titanium
The method of Al intermetallic coating.This method use Intermatallic Ti-Al compound target, generate coating ex situ generate and
The device is complicated.Xi'an engineering college, the Second Artillery Force (Li Ping) prepares Ti- in 45 steel surfaces using the method for Ultrasonic Arc Sprayed
Al coating (protect by microstructure and property research [J] material of Li Ping, Wang Hangong .45 steel surface resistance of supersonic wires arc sprayed Ti-Al composite coatings
Shield, 2002,35 (11): 12-14).This method causes anchoring strength of coating not high using spraying method, and Ti and Al are anti-at the same time
At once can not apply external pressure causes coating consistency little.Harbin Institute of Technology's college of materials science and engineering (Lv Zhijun)
Using plasma spraying method on Q235 steel fabricated in situ Ti-Al metal compound coatings (Lv Zhijun reaction and plasma spraying
Prepare research [D] the Harbin Institute of Technology of Ti-Al intermetallic compound composite coating, 2009).This method also has spraying
The defect of general character.Suitable auxiliary thermal source and pressuring method must be used by obtaining Ti-Al intermetallic compound coating in situ.This
A little methods are all not involved with the preparation method that high-frequency induction auxiliary self-spreading prepares TiAl system metal compound coatings.
Summary of the invention
Based on the above the deficiencies in the prior art, technical problem solved by the invention is to provide one kind directly in metal watch
Face prepares the high quality TiAl that smooth, fine and close, the porosity is low, bond strength is high by high-frequency induction auxiliary self-spreading method and applies
Layer.This method has the advantages that heating efficiency height and at low cost.
In order to solve the above technical problem, the present invention provides a kind of high-frequency induction auxiliary self-spreading TiAl system intermetallics
The preparation method of object coating, comprises the following steps:
(1) Ti powder and Al powder are mixed, acetone is then added, is stirred under 40~55 DEG C of ultrasound conditions, volatilized to acetone
Until stirring difficulty;Then vacuum drying treatment obtains mixing;Then steel mold bottom tiled it is dry after mixing,
It is pressed into the powder agglomates of compactness 50%~70%, is placed in spare in vacuum drying environment;
(2) matrix surface of steel plate is polished with sand paper and removes rusty stain, and is clean with washes of absolute alcohol, be put into seal box
It is spare;
(3) step (1) resulting powder agglomates is placed on above matrix steel plate, is put into graphite jig with latter piece;Then
It is reacted by high-frequency induction auxiliary self-spreading to get the high-frequency induction auxiliary self-spreading TiAl coating.
As a preferred embodiment of the above technical solution, high-frequency induction auxiliary self-spreading TiAl system provided by the invention intermetallic
The preparation method of object coating further comprises some or all of following technical characteristic:
As an improvement of the above technical solution, in the step (1), the partial size of Ti powder is 15~38 μm;The partial size of Al powder
It is 10~30 μm.
As an improvement of the above technical solution, in the step (1), Ti powder and Al powder press Ti/Al atomic ratio as 1:1~3
Ratio mixing.
As an improvement of the above technical solution, the condition of the vacuum drying treatment in the step (1) is 70~95 DEG C, very
Reciprocal of duty cycle < 133Pa, 10~15 hours of drying time;In step (1), it is placed in vacuum drying environment as at 70~95 DEG C, vacuum
It is 12~15 hours dry under the conditions of degree < 133Pa.
As an improvement of the above technical solution, before step (3) processing, in advance in graphite jig inner surface layer overlay
In addition graphite paper overlays Ti-Al mixed-powder below matrix;The Ti-Al mixed-powder is Ti powder and Al former by Ti/Al
Mixed-powder of the son than the ratio mixing for being 1:3.
As an improvement of the above technical solution, high-frequency induction auxiliary self-spreading reaction process described in step (3) is specifically such as
Under:
After sample is placed together with mold be put into induction coil middle cover upper box lid by hydraulic press to sample apply 2~
The precompression of 4MPa or so, opening simultaneously the logical argon gas of air valve makes box house reduce oxygen in cabinet full of argon gas for 1~5 minute
Content;450A electric current is selected to preheat 30s to sample later, about 300~400 DEG C of temperature measurer displays temperature, are closed later at this time
Power supply is uniform by specimen temperature, and power supply is opened after 5s using the electric current of 500~800A and continues heating until observing that reaction produces
Power supply is closed after raw thermal explosion, applies the pressure and 60~120s of pressure maintaining of 20~40MPa to sample immediately, subsequent sample is in argon gas
Natural cooling in environment.
Compared with prior art, technical solution of the present invention has the following beneficial effects:
The present invention directly prepares TiAl coating, TiAl obtained by high-frequency induction auxiliary self-spreading method in metal surface
Coating is smooth, fine and close, the porosity is low, bond strength is high.And the method for the present invention heating efficiency is high, at low cost.
The present invention is suitable for the surface peening of various tool and moulds and structural elements and remanufactures, and improves tool and mould and zero
The service life of part.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And it can be implemented in accordance with the contents of the specification, and in order to allow above and other objects, features and advantages of the invention can
It is clearer and more comprehensible, below in conjunction with preferred embodiment, detailed description are as follows.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, the attached drawing to embodiment is simply situated between below
It continues.
Fig. 1 is high-frequency induction auxiliary self-spreading schematic device used in the present invention;
Fig. 2 is high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating surface XRD obtained in embodiment 1
Figure;
Fig. 3 is high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating surface metallographic obtained in embodiment 1
Figure;
Fig. 4 is high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating profile scanning obtained in embodiment 1
Electron microscope.
Specific embodiment
The following detailed description of a specific embodiment of the invention, as part of this specification, by embodiment come
Illustrate that the principle of the present invention, other aspects of the present invention, feature and its advantage will become apparent by the detailed description.
Can be clearly seen that high-frequency induction auxiliary self-spreading device used in the present invention from Fig. 1: reaction chamber is used to accommodate stone
Black mold, graphite cylinder, induction coil, matrix steel and various powder;Argon gas is given from reaction lower box part before high-frequency induction heating
Entire reaction unit, which provides ar gas environment, prevents graphite jig, matrix steel and various powder in heating, reaction and cooling procedure
Oxidation;The graphite sleeve of graphite jig is used to accommodate graphite paper, matrix steel and reaction powder, and graphite sleeve heats up when high-frequency induction
Heat is provided to reaction powder and matrix, gives reaction unit to provide enclosed environment when pressurization;The graphite cylinder up and down of graphite jig
Reaction powder provides pressure and the heat of reaction system is prevented to scatter and disappear outward when for reaction;It is placed in around graphite sleeve
Induction coil is to graphite sleeve, matrix steel and reaction powder heating;The thermocouple for being placed in graphite sleeve lower part, which is used to measure, to be added
Temperature in heat and reaction process.
Industrial chemicals used in the present invention is technical grade product.
Embodiment 1
A kind of preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating, it includes following step
It is rapid:
(1) Ti powder and Al powder are mixed and is poured into beaker in the ratio that Ti/Al atomic ratio is 1:1 and stirred evenly, then
Acetone is poured into, beaker is placed on and continues to stir in supersonic wave cleaning machine, 50 DEG C of water temperature constant temperature, evaporating into stirring difficulty to acetone is
Only, hereafter beaker is put into vacuum oven again at a temperature of 85 DEG C, is dried in vacuo 12 hours;Then by the mixing after drying
It is put into mold, is pressed into the powder agglomates of compactness 55%, then place the powder agglomates pressed spare in a vacuum drying oven.
(2) 5CrTiMo surface of steel plate is polished with sand paper and removes rusty stain and other attachments, and is dry with washes of absolute alcohol
Only, it is put into spare in seal box.
(3) powder agglomates for preparing step 1 is placed on above 5CrNiMo steel plate, is put into graphite jig with latter piece;But
Additional Ti- is in addition also wanted below matrix in advance in graphite jig inner surface layer overlay graphite paper before being put into
75at.%Al mixed-powder is come the thermal loss for the system of supplementing;Induction coil middle cover is put into together with mold after sample is placed
Upper box lid applies the precompression of 2MPa or so by hydraulic press to sample, and opening simultaneously the logical argon gas of air valve makes box house in 2 minutes
The content of oxygen in cabinet is reduced full of argon gas;450A electric current is selected to preheat 30s to sample later, at this time temperature measurer displays temperature
About 300~400 DEG C, closing power supply is uniform by specimen temperature later, and power supply is opened after 5s and continues to add using the electric current of 600A
Heat closes power supply after observing the thermal explosion that reaction generates, and applies the pressure and pressure maintaining 120s of 30MPa to sample immediately, then
Sample natural cooling in an argon atmosphere.
Coating Phase Analysis: with X ' Pert PRO MPDX x ray diffractometer x (Cu-K α x-ray source, 0.02 ° of step-length, scanning range are 2 θ=10 °~90 °, scanning speed is 1.2 °/min) analysis composite coating
The object phase on surface.It is illustrated in figure 2 high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating obtained in embodiment 1
Surface XRD diagram, Cong Tuzhong is it may be seen that the object of coating surface is mutually TiAl3And Ti.
Coating morphology observations method: Axio Scope A1 (Carl Zeiss) type optical microphotograph sem observation coating surface is used
Metallographic microscope is illustrated in figure 3 high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating surface obtained in embodiment 1
Metallographic microscope, as can be seen from the figure coating surface is smooth, and quality is good.With the NOVA 400NanoSEM type with energy disperse spectroscopy
Field emission microscopy observation coating profile scanning electron microscope is illustrated in figure 4 the auxiliary of high-frequency induction obtained in embodiment 1 certainly
TiAl series intermetallic compound coating profile scanning electron microscope is spread, as can be seen from the figure the netted TiAl of Dark grey3It surrounds
Graininess Ti particle.
High-frequency induction self- propagating TiAl coating after above-mentioned process, has the effect that
(1) composite coating is smooth, fine and close, the porosity is low, bond strength is high.
(2) heating efficiency height and at low cost.
Embodiment 2
A kind of preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating, it includes following step
It is rapid:
(1) Ti powder and Al powder are mixed and is poured into beaker in the ratio that Ti/Al atomic ratio is 1:3 and stirred evenly, then
Acetone is poured into, beaker is placed on and continues to stir in supersonic wave cleaning machine, 55 DEG C of water temperature constant temperature, evaporating into stirring difficulty to acetone is
Only, hereafter beaker is put into vacuum oven again at a temperature of 95 DEG C, is dried in vacuo 11 hours;Then by the mixing after drying
It is put into mold, is pressed into the powder agglomates of compactness 60%, then place the powder agglomates pressed spare in a vacuum drying oven.
(2) H13 surface of steel plate is polished with sand paper and removes rusty stain and other attachments, and is clean with washes of absolute alcohol,
It is put into spare in seal box.
(3) powder agglomates for preparing step 1 is placed on above H13 steel plate, is put into graphite jig with latter piece;But it is being put into
Additional Ti-75at.%Al is in addition also wanted below matrix in advance in graphite jig inner surface layer overlay graphite paper before
Mixed-powder is come the thermal loss for the system of supplementing;Induction coil middle cover upper box lid is put into together with mold after sample is placed to pass through
Hydraulic press applies the precompression of 3MPa or so to sample, and opening simultaneously the logical argon gas of air valve subtracts box house full of argon gas in 4 minutes
The content of oxygen in few cabinet;Later select 450A electric current give sample preheat 30s, at this time temperature measurer displays temperature about 300~
400 DEG C, closing power supply is uniform by specimen temperature later, and power supply is opened after 5s using the electric current of 700A and continues heating until observing
Power supply is closed after the thermal explosion generated to reaction, applies the pressure and pressure maintaining 100s of 35MPa to sample immediately, subsequent sample is in argon gas
Natural cooling in environment.
High-frequency induction self- propagating TiAl coating after above-mentioned process, has the effect that
(1) composite coating is smooth, fine and close, the porosity is low, bond strength is high.
(2) heating efficiency height and at low cost.
Embodiment 3
A kind of preparation method of high-frequency induction auxiliary self-spreading TiAl coating, it includes the following steps:
(1) Ti powder and Al powder are mixed and is poured into beaker in the ratio that Ti/Al atomic ratio is 1:2 and stirred evenly, then
Acetone is poured into, beaker is placed on and continues to stir in supersonic wave cleaning machine, 45 DEG C of water temperature constant temperature, evaporating into stirring difficulty to acetone is
Only, hereafter beaker is put into vacuum oven again at a temperature of 70 DEG C, is dried in vacuo 15 hours;Then by the mixing after drying
It is put into mold, is pressed into the powder agglomates of compactness 70%, then place the powder agglomates pressed spare in a vacuum drying oven.
(2) No. 45 surface of steel plate are polished with sand paper and remove rusty stain and other attachments, and is clean with washes of absolute alcohol,
It is put into spare in seal box.
(3) powder agglomates for preparing step 1 is placed on above No. 45 steel plates, is put into graphite jig with latter piece;But it is putting
Additional Ti-75at.% is in addition also wanted below matrix in advance in graphite jig inner surface layer overlay graphite paper before entering
Al mixed-powder is come the thermal loss for the system of supplementing;Induction coil middle cover upper box lid is put into together with mold after sample is placed to lead to
The precompression that hydraulic press applies 4MPa or so to sample is crossed, opening simultaneously the logical argon gas of air valve makes box house full of argon gas for 5 minutes
Reduce the content of oxygen in cabinet;450A electric current is selected to preheat 30s to sample later, at this time temperature measurer displays temperature about 300
~400 DEG C, closing power supply is uniform by specimen temperature later, and power supply is opened after 5s using the electric current of 750A and continues heating until sight
Power supply is closed after observing the thermal explosion that reaction generates, applies the pressure and pressure maintaining 90s of 40MPa to sample immediately, subsequent sample is in argon
Natural cooling in compression ring border.
High-frequency induction self- propagating TiAl coating after above-mentioned process, has the effect that
(1) composite coating is smooth, fine and close, the porosity is low, bond strength is high.
(2) heating efficiency height and at low cost.
The bound of each raw material cited by the present invention and each raw material of the present invention, section value and technological parameter
Bound, the section value of (such as temperature, time) can realize the present invention, embodiment numerous to list herein.
The above is a preferred embodiment of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, it is noted that for those skilled in the art, without departing from the principle of the present invention, may be used also
To make several improvement and variation, these, which improve and change, is also considered as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating, which is characterized in that include
Following steps:
(1) Ti powder and Al powder are mixed, acetone is then added, is stirred under 40~55 DEG C of ultrasound conditions, evaporates into and stir to acetone
Until mixing difficulty;Then vacuum drying treatment obtains mixing;Then steel mold bottom tiled it is dry after mixing, compacting
At the powder agglomates of compactness 50%~70%, it is placed in spare in vacuum drying environment;
(2) matrix surface of steel plate is polished with sand paper and removes rusty stain, and is clean with washes of absolute alcohol, be put into standby in seal box
With;
(3) step (1) resulting powder agglomates is placed on above matrix steel plate, is put into graphite jig with latter piece;Then pass through
High-frequency induction auxiliary self-spreading reacts to get the high-frequency induction auxiliary self-spreading TiAl coating.
2. the preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating as described in claim 1,
Be characterized in that: in the step (1), the partial size of Ti powder is 15~38 μm;The partial size of Al powder is 10~30 μm.
3. the preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating as described in claim 1,
Be characterized in that: in the step (1), Ti powder and Al powder are mixed in the ratio that Ti/Al atomic ratio is 1:1~3.
4. the preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating as described in claim 1,
Be characterized in that: the condition of the vacuum drying treatment in the step (1) is 70~95 DEG C, vacuum degree < 133Pa, drying time 10
~15 hours;In step (1), being placed in vacuum drying environment is under the conditions of 70~95 DEG C, vacuum degree < 133Pa dry 12
~15 hours.
5. the preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating as described in claim 1,
It is characterized in that: before step (3) processing, in advance in graphite jig inner surface layer overlay graphite paper, in addition under matrix
Face overlays Ti-Al mixed-powder;The Ti-Al mixed-powder is that Ti powder and Al are mixed in the ratio that Ti/Al atomic ratio is 1:3
Mixed-powder.
6. the preparation method of high-frequency induction auxiliary self-spreading TiAl series intermetallic compound coating as described in claim 1,
Be characterized in that: high-frequency induction auxiliary self-spreading reaction process described in step (3) is specific as follows:
Induction coil middle cover upper box lid is put into together with mold after sample is placed, and the left side 2~4MPa is applied to sample by hydraulic press
Right precompression opens simultaneously air valve and leads to the content that argon gas makes box house reduce oxygen in cabinet full of argon gas for 1~5 minute;
It selects 450A electric current to preheat 30s to sample later, at this time about 300~400 DEG C of temperature measurer displays temperature, closes power supply later and allow
Specimen temperature is uniform, and power supply is opened after 5s using the electric current of 500~800A and continues heating until observing the heat that reaction generates
Power supply is closed after quick-fried, applies the pressure and 60~120s of pressure maintaining of 20~40MPa to sample immediately, subsequent sample is in an argon atmosphere
Natural cooling.
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CN114603143A (en) * | 2022-02-21 | 2022-06-10 | 中山大学 | Titanium steel composite board preparation method based on titanium-aluminum mixed intermediate layer |
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CN114603143B (en) * | 2022-02-21 | 2023-09-12 | 中山大学 | Titanium steel composite board preparation method based on titanium-aluminum mixed intermediate layer |
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