CN105780000B - A kind of preparation method of engine chamber surface recombination silicide coating - Google Patents

A kind of preparation method of engine chamber surface recombination silicide coating Download PDF

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Publication number
CN105780000B
CN105780000B CN201610305944.9A CN201610305944A CN105780000B CN 105780000 B CN105780000 B CN 105780000B CN 201610305944 A CN201610305944 A CN 201610305944A CN 105780000 B CN105780000 B CN 105780000B
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molybdenum
combustion chamber
target material
tungsten alloy
coating
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CN105780000A (en
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李海庆
陈道勇
徐方涛
贾中华
张绪虎
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
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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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/042—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
    • 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
    • C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
    • C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
    • C23C10/34—Embedding in a powder mixture, i.e. pack cementation
    • C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
    • C23C10/44—Siliconising
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • C23C28/048—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material with layers graded in composition or physical properties
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
    • F02K—JET-PROPULSION PLANTS
    • F02K9/00—Rocket-engine plants, i.e. plants carrying both fuel and oxidant therefor; Control thereof
    • F02K9/42—Rocket-engine plants, i.e. plants carrying both fuel and oxidant therefor; Control thereof using liquid or gaseous propellants
    • F02K9/60—Constructional parts; Details not otherwise provided for
    • F02K9/62—Combustion or thrust chambers

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • General Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to a kind of preparation methods of engine chamber surface recombination silicide coating, by being designed from the design of filtered cathode vacuum arc equipment inner surface cathode arc source and profiling molybdenum target material, thrust chamber combustion chamber surfaces externally and internally molybdenum coating preparation process, vacuum activating bag oozes dedicated crucible device design, vacuum activating bag oozes to form the optimization of molybdenum silicide coating process, the silication molybdenum coating of even compact is prepared in niobium alloy combustor surface, there are two types of profiling molybdenum target materials, a kind of is the molybdenum target material for depositing straightway to throat position, second is molybdenum target material of the throat to outlet port, the present invention realizes that engine operating temperature is increased to 1660 DEG C for the first time, improve the high temperature nargin of engine, extend engine life, the engine vacuum heat run service life reach 11 it is small when more than.

Description

A kind of preparation method of engine chamber surface recombination silicide coating
Technical field
The present invention relates to rail attitude control engine thrust chambers, are applied more particularly to a kind of combustion chamber in motor power chamber body portion Layer technology of preparing, and in particular to a kind of preparation method of engine chamber surface recombination silicide coating can be applied to space flight The engine of aircraft.
Background technology
Double elements liquid propellant rail control engine is the important composition of modern space aircraft and strategy and tactics weapon Part is widely used in orbits controlling, pose adjustment etc..In recent years, the development of course of new aircraft or weapon, to engine performance Requirement be continuously improved, it is desirable that its improve specific impulse, increase chamber pressure, so as to reduce the consumption of propellant and mitigate engine weight Amount and extension engine life or increase strategic arms range.Thrust chamber allowable temperature is the main of decision engine/motor specific impulse One of factor, and Thruster material and high-temperature oxidation resistant coating performance then determine the operating temperature and scour resistance of thrust chamber Energy.At present, China is applied to the importing of spacecraft track and the double elements liquid-propellant rocket engine of gesture stability mainly uses The niobium alloy of silicide coating makees Thruster material.For niobium hafnium-silicochromium titanium motor power room, matrix uses niobium hafnium alloy, Coating process and system are the silicochromium titanium coating of fused slurry and silicochromium titanium hafnium coating, and operating temperature is 1400 DEG C or so.
In order to further improve the service life of the engine jet pipe of the alloy at high temperature, according to silicide coating material Material, silication molybdenum coating can effectively improve niobium tungsten alloy high temperature oxidation resistance, and only Russia is this using molybdenum silicide at present Coating, but concrete structure and preparation process and method do not have external disclosure, especially motor power room entirety molybdenum silicide to apply Layer preparation scheme does not have any report.
The content of the invention
It is an object of the invention to overcome the above-mentioned deficiency of the prior art, a kind of engine chamber surface recombination silicon is provided The preparation method of compound coating system, coating prepared by this method enable the operating temperature of engine chamber to be increased to 1660 DEG C, the high temperature nargin of engine is improved, extends engine life.
What the above-mentioned purpose of the present invention was mainly achieved by following technical solution：
A kind of engine chamber, it is characterised in that：The engine chamber be niobium tungsten alloy combustion chamber, the niobium tungsten The internal face of alloy combustion chamber is equipped with compound silicide coating with outside wall surface, which includes the molybdenum silicide of outer layer Coating, the niobium disilicide layer in interlayer and three silication, the five niobium layer of bottom.
In above-mentioned engine chamber, the thickness of silication molybdenum coating is 90~150 μm, and the thickness of niobium disilicide layer is 20 ~50 μm, the thickness of three silication, five niobium layer is 5-15 μm.
In above-mentioned engine chamber, the boron that mass percentage content is 1~5% is contained in silication molybdenum coating.
A kind of preparation method of engine chamber surface recombination silicide coating, includes the following steps：
Step (1) deposits molybdenum coating in niobium tungsten alloy burning chamber internal surface, and specific method is as follows：
(1.1), the first molybdenum target material and the second molybdenum target material are prepared, wherein the first molybdenum target material is for the straight of niobium tungsten alloy combustion chamber Line segment to throat's inner surface molybdenum coating preparation, the second molybdenum target material for niobium tungsten alloy combustion chamber outlet section to throat's inner surface The preparation of molybdenum coating；
(1.2), the first molybdenum target material is mounted on inner surface vacuum cathode arc depositing device, as cathode, using electricity Magnetic field control arc spot moves up and down on the first molybdenum target material surface, by the way that size of current is controlled to control arc spot on the first molybdenum target material surface Upper-lower position, pass through the speed that curent change FREQUENCY CONTROL arc spot is controlled to move up and down on the first molybdenum target material surface；
(1.3), niobium tungsten alloy combustion chamber is placed, makes niobium tungsten alloy combustion chamber straightway downward, the first molybdenum target material is located at niobium Tungsten combustion chamber makes the axis of the first molybdenum target material be overlapped with niobium tungsten alloy burning chamber axis, and avoids the first molybdenum target material and niobium Tungsten alloy combustion chamber contacts, and niobium tungsten alloy combustion chamber is as anode；
(1.4), extract vacuum and control process conditions, complete niobium tungsten alloy combustion chamber straightway and applied to throat's inner surface molybdenum The deposition of layer；
(1.5), the second molybdenum target material is mounted on inner surface vacuum cathode arc depositing device, as cathode, using electricity Magnetic field control arc spot moves up and down on the second molybdenum target material surface, by the way that size of current is controlled to control arc spot on the second molybdenum target material surface Upper-lower position, pass through the speed that curent change FREQUENCY CONTROL arc spot is controlled to move up and down on the second molybdenum target material surface；
(1.6), niobium tungsten alloy combustion chamber is placed, makes niobium tungsten alloy combustor exit section downward, the second molybdenum target material is located at niobium Tungsten alloy combustion chamber makes the axis of the second molybdenum target material be overlapped with niobium tungsten alloy burning chamber axis, and avoids the second molybdenum target material It is contacted with niobium tungsten alloy combustion chamber, niobium tungsten alloy combustion chamber is as anode；
(1.7), extract vacuum and control process conditions, complete niobium tungsten alloy combustor exit section and applied to throat's inner surface molybdenum The deposition of layer；
Step (2), in niobium tungsten alloy combustion chamber outside deposition molybdenum coating；
Niobium tungsten alloy combustion chamber after step (3), deposition molybdenum coating carries out vacuum activating bag and oozes processing, is prepared compound Silicide coating system, specific method are as follows：
(3.1), bag bleed is fitted into graphite crucible, the embedment of niobium tungsten alloy combustion chamber is installed to the graphite crucible of bag bleed In, in the bag bleed for ensureing entire combustion chamber embedment graphite crucible；
(3.2), activator is fitted into activator evaporator；
(3.3), activator evaporator is packed into the first vacuum drying oven, graphite crucible is packed into the second vacuum drying oven, and even Logical activator evaporator and graphite crucible；
(3.4), carry out bag and ooze priming reaction formation silication molybdenum coating, specific method is：
First vacuum drying oven, the second vacuum drying oven vacuumize simultaneously, when vacuum degree reaches 2 × 10-2During below Pa, to the first vacuum Stove and the second vacuum drying oven are carried out at the same time heating, and the first vacuum drying oven firing rate is 8-10 DEG C/min, are heated to 880-960 DEG C, the Two vacuum drying oven firing rates are 15-20 DEG C/min, are heated to 1200-1400 DEG C, and two vacuum drying ovens are carried out with isothermal holding, heat preservation When time is 6-10 small, stove is then closed, and carries out furnace cooling, silication molybdenum coating is prepared.
In the preparation method of above-mentioned engine chamber surface recombination silicide coating, the first molybdenum target in step (1.1) Material shape and the straightway of niobium tungsten alloy combustion chamber match to throat's inner surface configuration, are segment+round platform+cylindrical shape, in Heart perforate；Second molybdenum target material shape and the outlet section of niobium tungsten alloy combustion chamber match to throat's inner surface configuration, also for segment+ Round platform+cylindrical shape, center drilling.
In the preparation method of above-mentioned engine chamber surface recombination silicide coating, step (1.2), step (1.5) Middle reference current control is 0.5-20A, and curent change refrequency control range is 3-10Hz.
In the preparation method of above-mentioned engine chamber surface recombination silicide coating, step (1.4), step (1.7) Middle extraction vacuum, vacuum gauge pressure≤6 × 10-2Below Pa starts to deposit molybdenum coating, and deposition process conditions are：Arc current 40-80A, 0.5~20A of coil current, frequency 3-10Hz.
In the preparation method of above-mentioned engine chamber surface recombination silicide coating, in niobium tungsten alloy in step (2) The concrete technology method of combustion chamber outside deposition molybdenum coating is as follows：
(2.1), vacuum the moon in outer surface will be mounted on for the 3rd molybdenum target material of niobium tungsten combustion chamber outside deposition molybdenum coating On pole electrical arc depositing device, as cathode；
(2.2), the niobium tungsten alloy combustion chamber for having deposited inner surface molybdenum coating is placed on outer surface vacuum cathode arc to sink On the stent of product equipment, the stent possesses up and down motion and rotation function；
(2.3), vacuum, vacuum gauge pressure≤6 × 10 are extracted-2Below Pa starts to deposit molybdenum coating, arc current 80-100A； Before depositing molybdenum coating, operating stent is opened, operating parameters are that up and down motion distance is 0-400mm, speed 1-5mm/s, rotation Speed is 0.5-3 circles/second.
In the preparation method of above-mentioned engine chamber surface recombination silicide coating, bag bleed includes in step (3) The mass ratio of silicon grain and boron powder, silicon grain and boron powder is：92~98：8~2；And silicon grain purity is more than 99.99%, grain size is in 0.5- Between 2mm；Boron powder purity is more than 99.95%, and grain size is between 100-300 μm.
In the preparation method of above-mentioned engine chamber surface recombination silicide coating, activator is halogen in step (3) Compound matter, is specially NaCl or KF, and the mass ratio of activator and bag bleed is：5~10：1000.
In the preparation method of above-mentioned engine chamber surface recombination silicide coating, graphite is used in step (3.3) Pipe connects activator evaporator and graphite crucible, and buffer substrate tablet of the molybdenum sheet as activator flow velocity is placed inside the graphite-pipe.
A kind of motor power room, includes above-mentioned engine chamber.
A kind of motor power room, the preparation method of the compound silicide coating of combustor surface uses in motor power room Above-mentioned preparation method.
The present invention has the advantages that compared with prior art：
It is (1), of the invention by being designed from the design of filtered cathode vacuum arc equipment inner surface cathode arc source and profiling molybdenum target material, Thrust chamber combustion chamber surfaces externally and internally molybdenum coating preparation process, vacuum activating bag ooze dedicated crucible device design, vacuum activating bag It oozes to form the optimization of molybdenum silicide coating process, the silication molybdenum coating of even compact is prepared in niobium alloy combustor surface, it is real for the first time Existing engine operating temperature is increased to 1660 DEG C.
(2), the present invention is imitative according to the feature design of burning chamber internal surface shape face from combustion chamber surfaces externally and internally work characteristics Shape High-Purity Molybdenum target, there are two types of the targets, and a kind of is the molybdenum target material for depositing straightway to throat position, is for second throat to going out The molybdenum target material of mouth position, then using filtered cathode vacuum arc technology, using inner surface cathode arc source, the spots moving in the arc source Control is controlled using electromagnetic field coil, by the electric current and conversion frequency of control coil, realizes arc spot in conical molybdenum target table Face Uniform Movement；Using the inner surface cathode arc source, straightway is carried out respectively to throat position and throat to the interior of outlet port Surface molybdenum coating deposition, the electromagnetism field current and sedimentation time during deposition are adjusted in deposition process, realizes table in combustion chamber The uniformity and compactness of face molybdenum coating, thickness can be controlled at 35~45 μm；
(3), the present invention oozes silicidation to post-depositional molybdenum coating progress vacuum packet, and the device that bag oozes activation is divided into instead Room and activator vaporization chamber are answered, silica flour, boron powder and combustion chamber product is placed for reative cell, places and live for activator vaporization chamber Agent, two cabins are connected with graphite-pipe, can realize and two rooms are controlled into trip temperature respectively, when controlling the reaction of reative cell Between and activator evaporation time and activator level, wherein inside the graphite-pipe using molybdenum sheet delaying as activator flow velocity Punching prevents that activator evaporation flow velocity is too fast, is readily burned room molybdenum coating and is reacted with silicon continuous uniform, finally obtain even compact Silication molybdenum coating；
(4), a large number of experiments show that, the combustion chamber of silication molybdenum coating that the present invention obtains enables the operating temperature of engine 1660 DEG C are enough increased to, significantly improves the specific impulse of engine and high temperature nargin, extends engine life, engine passes through vacuum Heat run is examined, the service life reach 11 it is small when more than, specific impulse reaches 319s, and high temperature nargin improves 100-150 DEG C.
Description of the drawings
Fig. 1 is niobium tungsten alloy combustion chamber schematic diagram of the present invention；
Fig. 2 is niobium tungsten alloy of the present invention burning chamber internal surface molybdenum target material schematic diagram；Wherein Fig. 2 a are the first molybdenum of the invention Target schematic diagram；Fig. 2 b are the second molybdenum target material schematic diagram of the invention.
Fig. 3 is niobium tungsten alloy of the present invention burning chamber internal surface arc deposited cathode arc source schematic diagram；
Fig. 4 is combustion chamber placement location schematic diagram when the first molybdenum target material and molybdenum coating of the invention deposit；
Fig. 5 is combustion chamber placement location schematic diagram when the second molybdenum target material and molybdenum coating of the invention deposit；
Fig. 6 oozes the whole graphite crucible device schematic diagram of reaction for vacuum activating bag of the present invention；
Fig. 7 oozes reaction process schematic diagram for vacuum activating bag of the present invention；
Fig. 8 is the compound silicide coating microphoto that the embodiment of the present invention 1 is prepared.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments：
It is niobium tungsten alloy combustion chamber schematic diagram of the present invention as shown in Figure 1；It is fired for niobium tungsten alloy inventive engine combustion chamber Room is burnt, internal face and the outside wall surface of niobium tungsten alloy combustion chamber form compound silicide coating system, the compound silicide coating body System includes the silication molybdenum coating of outer layer, the niobium disilicide layer in interlayer and three silication, the five niobium layer of bottom.Wherein silication molybdenum coating Thickness for 90~150 μm, the thickness of niobium disilicide layer is 20~50 μm, and the thickness of three silication, five niobium layer is 5-15 μm.It is described Contain the boron that mass percentage content is 1~5% in silication molybdenum coating.
The preparation method of the compound silicide coating system of inventive engine combustor surface, specifically comprises the following steps：
Step (1) deposits molybdenum coating in niobium tungsten alloy burning chamber internal surface, and specific method is as follows：
(1.1), according to target in combustion-chamber shape and two pure molybdenum (99.9at.%) cathodes of dimensioned profiling, One molybdenum target material 2 and the second molybdenum target material 5, molybdenum target material are machined using the superb molybdenum bar of melting, and purity is more than 99.99wt%. Wherein the first molybdenum target material 2 is used for the straightway of niobium tungsten alloy combustion chamber 1 to the preparation of throat's inner surface molybdenum coating, such as Fig. 2 a institutes Show, the second molybdenum target material 5 for niobium tungsten alloy combustion chamber 1 outlet section to throat's inner surface molybdenum coating preparation, as shown in Figure 2 b. First molybdenum target material 2 and the straightway of niobium tungsten alloy combustion chamber 1 match to throat's inner surface configuration, are segment+round platform+cylinder Shape, center drilling；Second molybdenum target material 5 and the outlet section of niobium tungsten alloy combustion chamber 1 match to throat's inner surface configuration, are also ball Lack+round platform+cylindrical shape, center drilling.
(1.2), it is illustrated in figure 3 niobium tungsten alloy burning chamber internal surface arc deposited cathode arc source schematic diagram of the present invention；It will First molybdenum target material 2 is mounted on inner surface vacuum cathode arc depositing device, and as cathode, the structure of the cathode is：It does not use Conventional permanent magnet control spots moving, but special electromagnetic field is used to control arc spot on 2 surface of the first molybdenum target material is uniform Lower movement, the electromagnetic field are generated using copper wire coil 7, which is wrapped in using the enameled wire of the high temperature in ure iron pipe, the paint The diameter 0.2-0.5mm of envelope curve, the winding number of turns are enclosed for 1000-2000, and arc spot is controlled in the first molybdenum by controlling size of current The upper-lower position on 2 surface of target, reference current control control arc spot in 0.5-20A by controlling curent change frequency The speed that one molybdenum target material surface moves up and down, for frequency in 3-10Hz, which is sine wave；The electromagnetic field of the cathode arc source 7 center of coil is passed through using ure iron pipe 6, and connects the first molybdenum target material 2, and effect is effective magnetic conduction.
(1.3), it is illustrated in figure 4 combustion chamber placement location schematic diagram when the first molybdenum target material and molybdenum coating of the invention deposit； By 1 straightway of niobium tungsten combustion chamber after drying downward, it is placed on vacuum chamber stent, the first molybdenum target material 2 is located in niobium tungsten combustion chamber 1 Portion makes the axis of the first molybdenum target material 2 be overlapped with 1 axis of niobium tungsten alloy combustion chamber, while avoids the first molybdenum target material 2 and niobium tungsten alloy Combustion chamber 1 contacts, and niobium tungsten alloy combustion chamber 1 is used as anode；
(1.4), vacuum, vacuum gauge pressure≤6 × 10 are extracted-2Below Pa starts to deposit molybdenum coating；Arc current is 40-80A, line 0.5~20A of loop current, frequency 3-10Hz；Sedimentation time is determined according to coating thickness requirement；Complete the burning of niobium tungsten alloy 1 straightway of room is to the deposition of throat's inner surface molybdenum coating.
(1.5), after the completion of the inner surface of straightway to throat position deposits molybdenum coating, combustion chamber 1 is cooled to vacuum chamber After 45 DEG C, open vacuum chamber and take out combustion chamber 1.
(1.6), the second molybdenum target material 5 is mounted on inner surface vacuum cathode arc depositing device, as cathode, the cathode Structure be：Conventional permanent magnet is not used to control spots moving, but special electromagnetic field is used to control arc spot in the second molybdenum 5 surface of target uniformly moves up and down, which is generated using copper wire coil, which is wrapped in using the enameled wire of the high temperature In ure iron pipe, the diameter 0.2-0.5mm of the enameled wire, the winding number of turns is enclosed for 1000-2000, is controlled by controlling size of current Arc spot 5 surface of the second molybdenum target material upper-lower position, reference current control in 0.5-20A, by control curent change frequency come The speed that control arc spot moves up and down on 5 surface of the second molybdenum target material, for frequency in 3-10Hz, which is sine wave；The moon The electromagnetic field lines circle center in polar arc source is passed through using ure iron pipe, and connects the second molybdenum target material 5, and effect is effective magnetic conduction.
(1.7), it is illustrated in figure 5 combustion chamber placement location schematic diagram when the second molybdenum target material and molybdenum coating of the invention deposit； By 1 outlet section of niobium tungsten combustion chamber of the good molybdenum coating of above-mentioned deposition downward, it is placed on vacuum chamber stent, the second molybdenum target material 5 is located at Inside niobium tungsten alloy combustion chamber 1, the axis of the second molybdenum target material 5 is made to be overlapped with 1 axis of niobium tungsten alloy combustion chamber, while avoids second Molybdenum target material 5 is contacted with niobium tungsten alloy combustion chamber 1, and niobium tungsten alloy combustion chamber 1 is used as anode.
(1.8), vacuum, vacuum gauge pressure≤6 × 10 are extracted-2Below Pa starts to deposit molybdenum coating；According to actual conditions, arc electricity It flows for 40-80A, 0.5~20A of coil current, frequency 3-10Hz；Sedimentation time is determined according to coating thickness requirement；It is complete Into 1 outlet section of niobium tungsten alloy combustion chamber to the deposition of throat's inner surface molybdenum coating；
(1.9), after the completion of the inner surface of outlet section to throat position deposits molybdenum coating, combustion chamber is cooled to 45 with vacuum chamber After DEG C, open vacuum chamber and take out combustion chamber.
Step (2), in 1 outside deposition molybdenum coating of niobium tungsten alloy combustion chamber；Specific method is as follows：
(2.1) the 3rd molybdenum electrode target oil removing for combustion chamber outside deposition molybdenum coating that will be designed and process Afterwards, on the vacuum cathode arc depositing device of outer surface, as cathode；3rd molybdenum target material is cylinder.
(2.2) combustion chamber 1 for having deposited inner surface molybdenum coating is placed to the branch of outer surface vacuum cathode arc depositing device On frame, which possesses up and down motion and rotation function；
(2.3) vacuum, vacuum gauge pressure≤6 × 10 are extracted-2Below Pa starts to deposit molybdenum coating；Before depositing molybdenum coating, open Stent is operated, operating parameters are that up and down motion distance is 0-400mm, and speed 1-5mm/s, rotational velocity is 0.5-3 circles/second； Arc current is 80-100A, and sedimentation time is determined according to coating thickness requirement；
(2.4) after the completion of outside deposition molybdenum coating, combustion chamber is cooled to less than 45 DEG C with vacuum chamber, opens vacuum chamber and takes Go out combustion chamber.
Niobium tungsten alloy combustion chamber (1) after step (3), deposition molybdenum coating carries out vacuum activating bag and oozes processing, is prepared Compound silicide coating system, specific method are as follows：
(3.1), vacuum packet oozes materials selection and mixing treatment
Using pure silicon grain and pure boron powder as raw material, suitable particle size and the silicon grain of ingredient qualification and boron powder are selected, is met true Sky activation bag oozes the basis of rear molybdenum silicide tungsten performance requirement.Bag bleed 12 includes the mass ratio of silicon grain and boron powder, silicon grain and boron powder For：92~98：8~2；And silicon grain purity is more than 99.99%, grain size is between 0.5-2mm；Boron powder purity is more than 99.95%, grain Footpath is between 100-300 μm.
By silica flour and boron powder according to 92~98：8~2 mass ratio carries out dispensing.Batch mixing and mill are carried out using ball-grinding machine Material processing, when processing time is 0.5-2 small.
(3.2), bag bleed 12, combustion chamber 1 and activator 13 are loaded
Bag bleed 12 is fitted into bag and oozed in graphite crucible 8 by (3.2.1), and the embedment of niobium tungsten alloy combustion chamber 1 is installed bag bleed In 12 graphite crucible 8, ensure that entire combustion chamber 1 is embedded in the bag bleed 12 of graphite crucible 8；If Fig. 6 is vacuum of the present invention work Change bag and ooze the whole graphite crucible device schematic diagram of reaction；Fig. 7 oozes reaction process schematic diagram for vacuum activating bag of the present invention.
(3.2.2), activator 13 is weighed, activator 13 is fitted into activator evaporator 9；Activator 13 is NaCl or KF Etc. halogenated substances, activator 13 and the mass ratio of bag bleed 12 be：5~10：1000.
(3.2.3), activator evaporator 9 is packed into the first vacuum drying oven, graphite crucible 8 is packed into the second vacuum drying oven, Activator evaporator 9 and graphite crucible 8 are connected using graphite-pipe 11,11 inside of graphite-pipe places molybdenum sheet 10 and is used as activator flow velocity Buffer substrate tablet.
(3.3), carry out bag and ooze priming reaction formation silication molybdenum coating, specific method is：
First vacuum drying oven, the second vacuum drying oven vacuumize simultaneously, when vacuum degree reaches 2 × 10-2During below Pa, to the first vacuum Stove and the second vacuum drying oven are carried out at the same time heating, and the first vacuum drying oven firing rate is 8-10 DEG C/min, are heated to 880-960 DEG C, the Two vacuum drying oven firing rates are 15-20 DEG C/min, are heated to 1200-1400 DEG C, and two vacuum drying ovens are carried out with isothermal holding, heat preservation When time is 6-10 small, stove is then closed, and carries out furnace cooling, silication molybdenum coating is prepared.
(3.4) sample is taken out
When vacuum packet, which oozes furnace temperature, is cooled to room temperature, graphite crucible 8 is taken out, the bag bleed 12 in crucible 8 is poured out, Combustion chamber product takes out, final to obtain molybdenum silicide coating burns room.
According to obtained engine chamber, motor power room is further obtained.
Embodiment 1
Using manufacture a kind of size asBody portion (For body portion minimum diameter,For Body portion maximum gauge, 200mm are body portion total length) exemplified by, illustrate the specific embodiment of the method for the present invention.
(a) combustion chamber part prepares
According to the drawing requirement in body portion, reserve with vehicle and welding surplus, difference Vehicle Processing combustion chamber (such as Fig. 1)；
(b) prepared by combustion chamber molybdenum coating
It uses following steps to prepare molybdenum coating in combustor surface：
(1) it is respectively straightway according to target (such as Fig. 2) in two pure molybdenum (99.9at.%) cathodes of drawing dimensioned To throat's inner surface with molybdenum target material and throat to outlet section inner surface target；
(2) by after the molybdenum target material oil removing of straightway to throat's inner surface, deposited mounted on inner surface vacuum cathode arc In equipment, as cathode；
(3) by the oil removing pickling of niobium tungsten combustion chamber, after drying, it is placed on vacuum chamber stent by combustion chamber straightway downward, protects Straightway is held to the molybdenum target material of throat's inner surface in the combustion chamber among hole, i.e., molybdenum target material axis is overlapped with burning chamber axis, together When target and combustion chamber is avoided to contact with each other, as shown in figure 4, combustion chamber workpiece is as anode；Throat and molybdenum target in the present embodiment The distance on material top is 10mm.
(4) vacuum, vacuum gauge pressure≤5 × 10 are extracted-2Below Pa starts to deposit molybdenum coating；According to actual conditions, arc current For 60A, 0.5~15A of coil current, frequency 5Hz；Sedimentation time is 60min, ensures the thickness of molybdenum coating at 45 μm；
(5) after the completion of the inner surface of straightway to throat position deposits molybdenum coating, combustion chamber is cooled to 45 DEG C with vacuum chamber Afterwards, open vacuum chamber and take out combustion chamber.
(6) by after the molybdenum target material oil removing of the inner surface of throat to outlet port, mounted on inner surface vacuum cathode arc On depositing device, as cathode；
(7) by the niobium tungsten combustor exit section of the good molybdenum coating of above-mentioned deposition downward, it is placed on vacuum chamber stent, keeps out To the molybdenum target material in the combustion chamber among hole of throat's inner surface, i.e., molybdenum target material axis is overlapped with the chamber axis that burns, and is kept away simultaneously for mouthful section Exempt from target and combustion chamber contacts with each other, as shown in figure 5, combustion chamber workpiece is as anode；Throat and molybdenum target material top in the present embodiment End distance is 3-5mm.
(8) vacuum, vacuum gauge pressure≤5 × 10 are extracted-2Below Pa starts to deposit molybdenum coating；According to actual conditions, arc current For 60A, 0.5~10A of coil current, frequency 5Hz；Sedimentation time is 35min, ensures the thickness of molybdenum coating at 45 μm；
(9) after the completion of the inner surface of outlet section to throat position deposits molybdenum coating, combustion chamber is cooled to 45 DEG C with vacuum chamber Afterwards, open vacuum chamber and take out combustion chamber.
(10) after the molybdenum electrode target oil removing for combustion chamber outside deposition molybdenum coating that will be designed and process, installation In outer surface vacuum cathodic arc deposition equipment, as cathode；
(11) combustion chamber for having deposited inner surface molybdenum coating is placed to the stent of outer surface vacuum cathode arc depositing device On, which possesses up and down motion and rotation function；
(12) vacuum, vacuum gauge pressure≤5 × 10 are extracted-2Below Pa starts to deposit molybdenum coating；Before depositing molybdenum coating, fortune is opened Turn stent, operating parameters are that up and down motion distance is 0-200mm, and speed 1mm/s, rotational velocity is 0.5 circle/second；Arc current For 80A, sedimentation time 8h, ensure the thickness of molybdenum coating at 30 μm；
(13) after the completion of outside deposition molybdenum coating, after combustion chamber is cooled to 45 DEG C with vacuum chamber, opens vacuum chamber and take out Combustion chamber.
(c) vacuum activating bag oozes processing
Niobium tungsten alloy combustion chamber after deposition molybdenum coating carries out the method that vacuum activating bag oozes processing, uses step such as Under：
(1) vacuum packet oozes materials selection and mixing treatment
Using pure silicon grain and pure boron powder as raw material, suitable particle size and the silicon grain of ingredient qualification and boron powder are selected, is met true Sky activation bag oozes the basis of rear molybdenum silicide tungsten performance requirement.Silicon grain selects purity to be more than 99.99%, and grain size is between 0.5-2mm； Boron powder selects purity to be more than 99.95%, and grain size is between 100-300 μm.
By silica flour and boron powder according to 950g：The mass ratio of 50g carries out dispensing.It is carried out using ball-grinding machine at batch mixing and abrasive material Reason, when processing time is 0.5 small.
(2) bag bleed, combustion chamber and activator are loaded, as shown in Figure 6,7.
I., the bag bleed prepared (silicon grain and boron powder) is fitted into the bag processed to ooze in graphite crucible, while by combustion chamber Embedment is installed in the graphite crucible of bag bleed, it is necessary to entire combustion chamber is embedded to bag bleed crucible, as shown in Figure 7.
II. activator is weighed, which is NaCl, quality 10g, which is packed into the work for designing and processing In agent evaporator.
III. activator evaporator being packed into evaporation heating, vacuum stove, bag oozes graphite crucible and is packed into reaction vacuum drying oven, Evaporator graphite crucible is connected with graphite-pipe and bag oozes reaction graphite crucible, and wait vacuumizes and heat reaction.
(3) carry out bag and ooze priming reaction formation silication molybdenum coating,
Vacuum packet is oozed stove to vacuumize, when vacuum degree reaches 1 × 10-2During Pa, the vacuum drying oven and bag of activator are oozed The vacuum drying oven of reaction is carried out at the same time heating, and the vacuum drying oven firing rate of activator is 10 DEG C/min, is heated to 900 DEG C, bag oozes anti- The vacuum drying oven firing rate answered is 15 DEG C/min, is heated to 1400 DEG C, carries out isothermal holding to two vacuum drying ovens, soaking time is 8 it is small when.Then stove is closed, and carries out furnace cooling.
(4) sample is taken out
When vacuum packet, which oozes furnace temperature, is cooled to room temperature, graphite crucible is taken out, the bag bleed in crucible is poured out, burning Room product takes out, final to obtain.
The compound silicide coating microphoto that the embodiment of the present invention 1 is prepared is illustrated in figure 8, as seen from the figure The compound silicide coating outermost layer being prepared is MoSi2, interlayer NbSi2, bottom Nb5Si3。
Testing surface：The operating temperature of engine is enable to be increased to 1660 DEG C, significantly improve engine specific impulse and High temperature nargin, extend engine life, engine by vacuum heat run examination, the service life reach 11 it is small when more than, specific impulse reaches 319s, high temperature nargin improve 100-150 DEG C.
The above is only the optimal specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, Any one skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in, It should be covered by the protection scope of the present invention.
The content not being described in detail in description of the invention belongs to the known technology of professional and technical personnel in the field.

Claims (9)

1. a kind of preparation method of engine chamber surface recombination silicide coating, it is characterised in that：Include the following steps：
Step (1) deposits molybdenum coating in niobium tungsten alloy burning chamber internal surface, and specific method is as follows：
(1.1), the first molybdenum target material (2) and the second molybdenum target material (5) are prepared, wherein the first molybdenum target material (2) burns for niobium tungsten alloy To the preparation of throat's inner surface molybdenum coating, the second molybdenum target material (5) goes out the straightway of room (1) for niobium tungsten alloy combustion chamber (1) Mouthful section is to the preparation of throat's inner surface molybdenum coating；
(1.2), the first molybdenum target material (2) is mounted on inner surface vacuum cathode arc depositing device, as cathode, using electromagnetism Field control arc spot moves up and down on the first molybdenum target material (2) surface, by the way that size of current is controlled to control arc spot in the first molybdenum target material (2) The upper-lower position on surface passes through the speed that curent change FREQUENCY CONTROL arc spot is controlled to move up and down on the first molybdenum target material (2) surface；
(1.3), niobium tungsten alloy combustion chamber (1) is placed, makes niobium tungsten alloy combustion chamber (1) straightway downward, the first molybdenum target material (2) position In niobium tungsten combustion chamber, the axis of the first molybdenum target material (2) is made to be overlapped with niobium tungsten alloy combustion chamber (1) axis, and avoids first Molybdenum target material (2) is contacted with niobium tungsten alloy combustion chamber (1), and niobium tungsten alloy combustion chamber (1) is used as anode；
(1.4), extract vacuum and control process conditions, complete niobium tungsten alloy combustion chamber (1) straightway and applied to throat's inner surface molybdenum The deposition of layer；
(1.5), the second molybdenum target material (5) is mounted on inner surface vacuum cathode arc depositing device, as cathode, using electromagnetism Field control arc spot moves up and down on the second molybdenum target material (5) surface, by the way that size of current is controlled to control arc spot in the second molybdenum target material (5) The upper-lower position on surface passes through the speed that curent change FREQUENCY CONTROL arc spot is controlled to move up and down on the second molybdenum target material (5) surface；
(1.6), niobium tungsten alloy combustion chamber (1) is placed, makes niobium tungsten alloy combustion chamber (1) outlet section downward, the second molybdenum target material (5) position It is internal in niobium tungsten alloy combustion chamber (1), the axis of the second molybdenum target material (5) is made to be overlapped with niobium tungsten alloy combustion chamber (1) axis, and is kept away Exempt from the second molybdenum target material (5) to contact with niobium tungsten alloy combustion chamber (1), niobium tungsten alloy combustion chamber (1) is used as anode；
(1.7), extract vacuum and control process conditions, complete niobium tungsten alloy combustion chamber (1) outlet section and applied to throat's inner surface molybdenum The deposition of layer；
Step (2), in niobium tungsten alloy combustion chamber (1) outside deposition molybdenum coating；
Niobium tungsten alloy combustion chamber (1) after step (3), deposition molybdenum coating carries out vacuum activating bag and oozes processing, is prepared compound Silicide coating system, specific method are as follows：
(3.1), bag bleed (12) is fitted into graphite crucible (8), niobium tungsten alloy combustion chamber (1) embedment is installed into bag bleed (12) Graphite crucible (8) in, ensure entire combustion chamber (1) be embedded to graphite crucible (8) bag bleed (12) in；
(3.2), activator (13) is fitted into activator evaporator (9)；
(3.3), activator evaporator (9) is packed into the first vacuum drying oven, graphite crucible (8) is packed into the second vacuum drying oven, and Connect activator evaporator (9) and graphite crucible (8)；
(3.4), carry out bag and ooze priming reaction formation silication molybdenum coating, specific method is：
First vacuum drying oven, the second vacuum drying oven vacuumize simultaneously, when vacuum degree reaches 2 × 10-2During below Pa, to the first vacuum drying oven and Second vacuum drying oven is carried out at the same time heating, and the first vacuum drying oven firing rate is 8-10 DEG C/min, is heated to 880-960 DEG C, and second is true Empty stove heat speed is 15-20 DEG C/min, is heated to 1200-1400 DEG C, and isothermal holding, soaking time are carried out to two vacuum drying ovens For 6-10 it is small when, then close stove, and carry out furnace cooling, silication molybdenum coating be prepared；
The engine chamber is niobium tungsten alloy combustion chamber, and internal face and the outside wall surface of the niobium tungsten alloy combustion chamber are equipped with again Silicide coating is closed, which includes the silication molybdenum coating of outer layer, the niobium disilicide layer in interlayer and bottom Three silication, five niobium layer.
2. a kind of preparation method of engine chamber surface recombination silicide coating according to claim 1, feature It is：The straightway of the first molybdenum target material (2) shape and niobium tungsten alloy combustion chamber (1) is to throat's inner surface in the step (1.1) Shape matches, for segment+round platform+cylindrical shape, center drilling；Second molybdenum target material (5) shape and niobium tungsten alloy combustion chamber (1) Outlet section match to throat's inner surface configuration, be also segment+round platform+cylindrical shape, center drilling.
3. a kind of preparation method of engine chamber surface recombination silicide coating according to claim 1, feature It is：Reference current control is 0.5-20A in the step (1.2), step (1.5), and curent change refrequency control range is 3- 10Hz。
4. a kind of preparation method of engine chamber surface recombination silicide coating according to claim 1, feature It is：Vacuum, vacuum gauge pressure≤6 × 10 are extracted in the step (1.4), step (1.7)-2Below Pa starts to deposit molybdenum coating, Deposition process conditions are：Arc current 40-80A, 0.5~20A of coil current, frequency 3-10Hz.
5. a kind of preparation method of engine chamber surface recombination silicide coating according to claim 1, feature It is：It is as follows in the concrete technology method of niobium tungsten alloy combustion chamber (1) outside deposition molybdenum coating in the step (2)：
(2.1), the 3rd molybdenum target material that will be used for niobium tungsten combustion chamber (1) outside deposition molybdenum coating is mounted on outer surface vacuum cathode In arc deposited equipment, as cathode；
(2.2), the niobium tungsten alloy combustion chamber (1) for having deposited inner surface molybdenum coating is placed on outer surface vacuum cathode arc deposition On the stent of equipment, the stent possesses up and down motion and rotation function；
(2.3), vacuum, vacuum gauge pressure≤6 × 10 are extracted-2Below Pa starts to deposit molybdenum coating, arc current 80-100A；Deposition Before molybdenum coating, operating stent is opened, operating parameters are that up and down motion distance is 0-400mm, speed 1-5mm/s, rotational velocity For 0.5-3 circles/second.
6. a kind of preparation method of engine chamber surface recombination silicide coating according to claim 1, feature It is：Bag bleed (12) includes silicon grain and boron powder in the step (3), and the mass ratio of silicon grain and boron powder is：92~98：8~2； And silicon grain purity is more than 99.99%, grain size is between 0.5-2mm；Boron powder purity be more than 99.95%, grain size 100-300 μm it Between.
7. a kind of preparation method of engine chamber surface recombination silicide coating according to claim 1, feature It is：Activator (13) is halogenated substances in the step (3), is specially the mass ratio of NaCl or KF, activator and bag bleed For：5~10：1000.
8. a kind of preparation method of engine chamber surface recombination silicide coating according to claim 1, feature It is：Activator evaporator (9) and graphite crucible (8), the graphite-pipe are connected using graphite-pipe (11) in the step (3.3) (11) the internal buffer substrate tablet for placing molybdenum sheet (10) as activator flow velocity.
9. a kind of motor power room, it is characterised in that：The compound silicide coating of combustor surface in the motor power room Preparation method using preparation method as described in claim 1~8 any one.
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CN107955931A (en) * 2017-11-21 2018-04-24 西安航天发动机厂 Vertical high-temperature vacuum packet oozes stove
CN112921293A (en) * 2021-02-01 2021-06-08 航天材料及工艺研究所 High-silicon molybdenum silicide composite gradient coating on inner and outer surfaces of engine thrust chamber body and preparation method thereof

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