CN108588650B - Vacuum cathode arc source device and coating deposition method - Google Patents

Vacuum cathode arc source device and coating deposition method Download PDF

Info

Publication number
CN108588650B
CN108588650B CN201810384095.XA CN201810384095A CN108588650B CN 108588650 B CN108588650 B CN 108588650B CN 201810384095 A CN201810384095 A CN 201810384095A CN 108588650 B CN108588650 B CN 108588650B
Authority
CN
China
Prior art keywords
coating
spray pipe
section
arc
vacuum
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201810384095.XA
Other languages
Chinese (zh)
Other versions
CN108588650A (en
Inventor
李海庆
陈道勇
徐方涛
闫旭波
张绪虎
贾中华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
Original Assignee
China Academy of Launch Vehicle Technology CALT
Aerospace Research Institute of Materials and Processing Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Academy of Launch Vehicle Technology CALT, Aerospace Research Institute of Materials and Processing Technology filed Critical China Academy of Launch Vehicle Technology CALT
Priority to CN201810384095.XA priority Critical patent/CN108588650B/en
Publication of CN108588650A publication Critical patent/CN108588650A/en
Application granted granted Critical
Publication of CN108588650B publication Critical patent/CN108588650B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • 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
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C23C14/046—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
    • 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

Landscapes

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

Abstract

The invention relates to a vacuum cathode arc source device and a method for depositing a coating on the inner surface of a rocket engine spray pipe, in particular to the vacuum cathode arc source device and the method for depositing the coating on the inner surface of an on-orbit attitude control engine spray pipe, which can be applied to a two-component liquid rocket orbit/attitude control engine of an aerospace craft. The invention realizes the deposition of the protective coating on the inner surface of the track attitude control engine spray pipe by using a vacuum cathode arc ion deposition method, and can deposit different coatings such as a pure metal coating (an iridium coating, a rhenium coating, a niobium coating and a molybdenum coating) and an alloy coating (a platinum-rhodium coating, a Mo-W coating and a MCrAlYSiB coating) according to requirements, thereby improving the working performance of the track attitude control engine.

Description

Vacuum cathode arc source device and coating deposition method
Technical Field
The invention relates to a vacuum cathode arc source device and a method for depositing a coating on the inner surface of a rocket engine spray pipe, in particular to the vacuum cathode arc source device and the method for depositing the coating on the inner surface of an on-orbit attitude control engine spray pipe, which can be applied to a two-component liquid rocket orbit/attitude control engine of an aerospace craft.
Background
The bipropellant liquid propellant rail attitude control engine is an important component of modern space vehicles and strategic tactical weapons, and is widely applied to rail control, attitude adjustment and the like.
In recent years, the development of new aircrafts or weapons has increasingly required the performance of engines, which requires an increase in the specific impulse and an increase in the chamber pressure, thereby reducing the consumption of propellants and the weight of the engines, as well as prolonging the life of the engines or increasing the range of the strategic weapons. The allowable temperature of the nozzle is one of the main factors for determining the specific impulse of the engine, and the performance of the nozzle material and the protective coating on the inner surface of the nozzle determine the performance such as the working temperature, the service life and the like of the engine.
The base material of the bipropellant liquid propellant rail attitude control engine nozzle for guiding in the spacecraft rail and controlling the attitude is generally niobium alloy, the coating system is a silicon-chromium-titanium material system, and the preparation method mainly adopts a slurry sintering method. The engine working temperature of the coating system and the preparation method is below 1400 ℃, and the high performance requirement of a new generation of engine cannot be met.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the defects in the prior art are overcome, and a vacuum cathode arc source device and a method for depositing a coating on the inner surface of a rocket engine nozzle are provided, wherein the method can realize the following steps: phi 10-50mm, length of nozzle: 5-200 mm; inner surface coating thickness: 100-300 μm; coating thickness deposition rate of inner surface: 1-5 μm/min coating deposition method, the type of the deposited coating: the pure metal coating (iridium coating, rhenium coating, niobium coating and molybdenum coating) and the alloy coating (Mo-W coating, Nb-W coating, Hf-Ta coating and MCrAlYSiB coating) improve the high-temperature margin of the engine and prolong the service life of the engine.
The technical solution of the invention is as follows:
a vacuum cathode arc source device comprises a cathode target, a non-magnetic stainless steel auxiliary anode, a non-contact high-voltage pulse arc striking, a cooling water pipe, a mandrel and an electromagnetic coil;
the cathode target is made of iridium, rhenium, niobium, molybdenum, Mo-W, Nb-W, Hf-Ta or MCrAlYSiB;
when the inner diameter of the spray pipe is more than 20mm, the cathode target comprises a hollow cylindrical section and a hollow conical section; the top end of the conical section is an arc transition section which is matched with (is in a shape of) the convergent section of the spray pipe; the conical section is positioned above the cylindrical section, and the included angle between the generatrix of the conical section and the central axis of the conical section is 8-13 degrees; the inner surface of the cylindrical section is provided with internal threads, the height of the cylindrical section is 8-10mm, the height of the conical section is h, the length from the nozzle opening to the throat is L, h is L-d, and d is 5-8;
when the inner diameter of the spray pipe is less than or equal to 20mm, a hollow transition section is arranged between the cylindrical section and the conical section; the height of the transition section is 20-25 mm;
the non-magnetic stainless steel auxiliary anode is a hollow cylinder, the inner diameter of the hollow cylinder is 10-15mm larger than the maximum outer diameter of the cathode target material, and the outer diameter of the hollow cylinder is 50-60 mm; the height of the hollow cylinder is consistent with that of the cylinder section of the cathode target material; the side surface of the non-magnetic stainless steel auxiliary anode is provided with a threaded through hole;
the non-contact high-voltage pulse arc striking device comprises a copper core, a ceramic sleeve and a molybdenum sleeve, wherein the ceramic sleeve is sleeved outside the copper core, the molybdenum sleeve is sleeved outside the ceramic sleeve, the diameter of the copper core is 2-3mm, the length of the copper core is 10-20mm larger than that of the ceramic sleeve, the inner diameter of the ceramic sleeve is matched with that of the copper core, the length of the ceramic sleeve is 30-35mm, the outer diameter of the ceramic sleeve is 10-12mm, the inner diameter of the molybdenum sleeve is matched with that of the ceramic sleeve, the length of the molybdenum sleeve is 10-15mm smaller than that of the ceramic sleeve, and the wall thickness of the molybdenum sleeve is 1-3 mm; the outer surface of the molybdenum sleeve is provided with external threads;
the material of the mandrel is a magnetic conductive material with low remanence, such as pure iron; the mandrel is a hollow cylinder, the outer surface of the top end of the mandrel is provided with external threads, and the wall thickness of the mandrel is 3-5 mm; the outer diameter of the mandrel is 20-25 mm;
the electromagnetic coil is made of high-temperature-resistant enameled copper wires in a winding mode, the winding number is 500-fold and 800-fold, the height is 100-fold and 150mm, and the inner diameter of the electromagnetic coil is matched with the outer diameter of the mandrel;
the electromagnetic coil is wound outside the mandrel, one end of the mandrel is connected with the cathode, the other end of the mandrel is connected with the cylindrical section at the bottom end of the cathode target through threads, and the cooling water pipe penetrates through the mandrel and then extends to the conical section at the top end of the cathode target; the non-magnetic stainless steel auxiliary anode is sleeved on the outer surface of the cylindrical section of the cathode target material; the non-contact high-voltage pulse arc striking is fixedly connected with the non-magnetic stainless steel auxiliary anode through a threaded through hole on the side surface of the non-magnetic stainless steel auxiliary anode; the distance between the end surface of the copper core of the non-contact high-voltage pulse arc striking and the outer surface of the cylindrical section of the cathode target material is 1-2 mm.
A method for depositing a coating on an interior surface of a rocket motor nozzle using a vacuum cathodic arc source device, the method comprising the steps of:
(1) placing a cathode target material, a non-magnetic stainless steel auxiliary anode and a non-contact high-voltage pulse arc striking in a vacuum cathode arc source device into a vacuum chamber, wherein an electromagnetic coil is positioned outside the vacuum chamber, one part of a cooling water pipe and a mandrel is positioned in the vacuum chamber, and the other part of the cooling water pipe and the mandrel is positioned outside the vacuum chamber;
(2) cleaning the inner surface of the spray pipe; cleaning by acid washing and acetone ultrasonic cleaning, and drying;
(3) sleeving the spray pipe cleaned in the step (2) on the outer surface of the cathode target material in the step (1), and vacuumizing a vacuum chamber; the spray pipe is coaxial with the cathode target material, and the inner surface of the spray pipe is not contacted with the cathode target material; the conical sections of the cathode target are all positioned in the spray pipe;
(4) when the vacuum degree is less than 5 multiplied by 10-2When Pa, depositing a coating on the inner surface of the spray pipe by using an arc deposition method;
(5) and after the deposition of the coating is finished, cooling for more than 3 hours under the vacuum condition, and then taking out the spray pipe to obtain the spray pipe with the coating deposited on the inner surface.
In the step (4), the arc deposition process parameters are as follows: the current of the electromagnetic coil is direct current, the current adopts triangular waves, the amplitude is 0.2-15A, the frequency of the current is 1-5Hz, the moving distance and height of the arc spot on the surface of the cathode target material are realized by adjusting the amplitude of the current, and the up-and-down moving speed of the arc spot on the surface of the cathode target material is controlled by controlling the frequency of the current; the arc current of the arc deposition is 40-80A; the thickness of the deposited coating is 100-200 μm.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention designs a vacuum cathode arc source and a deposition method which accord with the deposition coating on the inner surface of the engine spray pipe from the characteristics of the inner surface of the engine spray pipe. The problem of difficult deposition of the coating on the inner surface of the engine spray pipe of the orbital attitude control is solved by the design of a vacuum cathode arc source, including the design of an electromagnetic field for controlling the motion of cathode arc spots, the design of a non-contact cathode target arc striking structure, the design of a profiling cathode target and the auxiliary anode of the arc source. The vacuum arc cathode arc source is utilized to deposit a protective coating on the inner surface of the spray pipe, the coating deposition process is optimized, the arc current, the electromagnetic current, the deposition time and the like are mainly included, the high-quality protective coating deposition on the inner surface of the spray pipe of the engine is realized, the coating thickness is more than 100 micrometers, and the coating is compact and has good adhesive force.
(2) A large number of tests show that the method can realize the following nozzle inner hole diameters: phi 10-50mm, length of nozzle: 5-200 mm; inner surface coating thickness: 100-; coating thickness deposition rate of inner surface: 1-5 μm/min coating deposition method, the type of the deposited coating: the pure metal coating (iridium coating, rhenium coating, niobium coating and molybdenum coating) and the alloy coating (Mo-W coating, Nb-W coating, Hf-Ta coating and MCrAlYSiB coating) improve the high-temperature margin of the engine and prolong the service life of the engine.
At present, the disclosed coating preparation process and vacuum arc deposition system can not realize the deposition of the coating on the inner surface of the engine spray pipe, particularly the size of the spray pipe is as follows: diameter of the inner hole of the spray pipe: phi 10-50mm, length of nozzle: 5-200 mm; coating thickness of inner surface of track attitude control engine nozzle: 100-300 μm; coating thickness deposition rate of inner surface: 1-5 μm/min.
The kind of the deposited coating is as follows: pure metal coatings (iridium, rhenium, niobium and molybdenum), alloy coatings (Mo-W, Nb-W, Hf-Ta, MCrAlYSiB).
In order to improve the working temperature of the engine and prolong the service life of the engine, a new coating deposition method of a vacuum arc source needs to be designed, so that the preparation of a coating with more excellent performance on the inner surface of the spray pipe is realized, and particularly, the high-quality protective coating with smooth and compact inner surface of the spray pipe and excellent adhesive force is realized.
(3) The invention provides a vacuum cathode arc source and a deposition method for depositing a coating on the inner surface of a spray pipe, aiming at the spray pipe of a rail attitude control engine spray pipe. The problem of difficult deposition of the coating on the inner surface of the engine spray pipe of the orbital attitude control is solved by the design of a vacuum cathode arc source, including the design of an electromagnetic field for controlling the motion of cathode arc spots, the design of a non-contact cathode target arc striking structure, the design of a profiling cathode target and the auxiliary anode of the arc source. The vacuum arc cathode arc source is utilized to deposit a protective coating on the inner surface of the spray pipe, the coating deposition process is optimized, the arc current, the electromagnetic current, the deposition time and the like are mainly included, the high-quality protective coating deposition on the inner surface of the spray pipe of the engine is realized, the coating thickness is more than 100 micrometers, and the coating is compact and has good adhesive force.
The invention realizes the deposition of the protective coating on the inner surface of the track attitude control engine spray pipe by using a vacuum cathode arc ion deposition method for the first time, and different coatings such as a pure metal coating (an iridium coating, a rhenium coating, a niobium coating and a molybdenum coating) and an alloy coating (a platinum-rhodium coating, a Mo-W coating and a MCrAlYSiB coating) can be deposited according to requirements, so that the working performance of the track attitude control engine is improved.
Drawings
FIG. 1 is a schematic structural view of a nozzle of a two-component liquid rocket rail attitude control engine according to the present invention;
FIG. 2 is a schematic view of the vacuum cathode arc source apparatus according to the present invention;
FIG. 3 is a schematic illustration of an inner surface coating of the present invention deposited in a straight section through the throat of an engine nozzle;
FIG. 4 is a schematic illustration of the deposition of an inner surface coating of the nozzle throat to the outlet section of the engine of the present invention;
FIG. 5 is a graph showing the results of thickness measurement and microscopic analysis of the nozzle of example 1;
FIG. 6 is a graph showing the results of thickness measurement and microscopic analysis of the nozzle of example 2.
Detailed Description
A vacuum cathode arc ion deposition method for an inner surface coating of an orbital control engine spray pipe is disclosed, and a vacuum cathode arc ion deposition arc source is used for depositing a high-temperature protective coating on the inner surface of the orbital control engine spray pipe.
The size of the rail attitude control engine spray pipe product is as follows: diameter of the inner hole of the spray pipe: phi 10-50mm, length of nozzle: 5-200 mm. Coating thickness of inner surface of track attitude control engine nozzle: 100-300 μm.
(1) The arc source of vacuum cathode arc ion deposition adopts a novel non-contact high-voltage pulse arc striking.
(2) The arc spot movement on the surface of the cathode target material is controlled by adopting an electromagnetic field, the current adopts triangular waves, the amplitude is 0.2-15A, and the frequency is 1-5 Hz. The moving distance and height of the arc spot on the surface of the target material are realized by adjusting the amplitude of the current, and the up-and-down moving speed and etching time of the arc spot on the surface of the cathode target material are controlled by controlling the current change frequency.
(3) The cathode target is designed into a hollow spray pipe profiling cylindrical conical target, a high magnetic conduction pipe material is arranged inside the cathode target, and an electromagnetic field is guided to the surface of the cylindrical conical target through the high magnetic conduction material.
(4) A non-magnetic stainless steel cover is arranged below the cathode target material and is used for providing an auxiliary anode and shielding a gap with the target material.
(5) The spray pipe is used as a workpiece for depositing the coating and is also used as an arc source anode.
A vacuum cathode arc ion deposition method for depositing a coating on the inner wall of an engine spray pipe comprises the following steps:
(1) the vacuum cathode arc ion source can be in high vacuum (vacuum degree is less than or equal to 3 multiplied by 10)-3Pa), the deposition of the metal coating on the inner surface of the spray pipe can be realized.
(2) Realizing the deposition rate of the thickness of the coating on the inner surface of the track attitude control engine spray pipe: 1-5 μm/min.
(3) The thickness of the coating on the inner surface of the track attitude control engine spray pipe is realized: 100-300 μm.
(4) The cathode material is evaporated and ionized by vacuum pulsed arc discharge to form a pure plasma which, after deposition on the substrate surface, forms the desired coating. Only pure plasma is generated in the whole process, and the coating has stable performance, smoothness, compactness and excellent adhesive force.
FIG. 1 is a schematic view of a two-component liquid rocket rail/attitude control engine nozzle having a variable cross-section configuration.
FIG. 2 shows a vacuum cathode arc source for preparing the inner surface coating of the orbital control engine nozzle, which solves the problem of difficult deposition of the inner surface coating of the orbital control engine nozzle through the design of the vacuum cathode arc source, including the electromagnetic field design for controlling the motion of cathode arc spots, the non-contact type cathode target arc striking structure design, the profiling cathode target design and the arc source auxiliary anode. The diameter of the inner hole of the spray pipe can be realized: phi 10-50mm, length of nozzle: 5-200 mm; inner surface coating thickness: 100-300 μm; the uniformity of the coating thickness is +/-10 microns; coating thickness deposition rate of inner surface: 1-5 μm/min coating deposition method, the type of the deposited coating: pure metal coatings (iridium, rhenium, niobium and molybdenum), alloy coatings (Mo-W, Nb-W, Hf-Ta, MCrAlYSiB).
The invention discloses a preparation method of a vacuum cathode arc source for depositing a coating on the inner surface of an engine spray pipe, which comprises the following steps:
(1) FIG. 3 is a schematic view of an arc deposition cathode arc source for an internal surface of an engine nozzle in a straight section to throat position in accordance with the present invention; the structure of the cathode is as follows: 1. the arc source of vacuum cathode arc ion deposition adopts a novel non-contact high-voltage pulse arc striking. 2. The arc spot movement on the surface of the cathode target material is controlled by adopting an electromagnetic field, the current waveform adopts triangular waves, the amplitude is 0.2-15A, and the frequency is 1-5 Hz. The moving distance and height of the arc spot on the surface of the target material are realized by adjusting the amplitude of the current, and the up-and-down moving speed and etching time of the arc spot on the surface of the cathode target material are controlled by controlling the current change frequency. 3. The cathode target is designed into a hollow spray pipe profiling cylindrical conical target, a high magnetic conduction pipe material is arranged inside the cathode target, and an electromagnetic field is guided to the surface of the cylindrical conical target through the high magnetic conduction material. 4. A non-magnetic stainless steel cover is arranged below the cathode target material and is used for providing an auxiliary anode and shielding a gap with the target material. 5. The spray pipe is used as a workpiece for depositing the coating and is also used as an arc source anode.
(2) And processing a profiling metal cathode inner target according to the shape and the size of the engine spray pipe, wherein the metal target is matched with the shape of the inner surface of the engine spray pipe, is in a spherical segment, round table and cylindrical shape, and is provided with a hole at the center. The principle of designing the shape of the cathode target according to the shape of the inner surface of the spray pipe is to design a profiling target according to the shape of the spray pipe, and the surface size of the target is 5-8mm smaller than the size of the inner surface of the spray pipe. The machined target was mounted onto a vacuum arc cathode arc source as shown in fig. 2. And (3) arcing the target material, wherein the arcing time is 5-10min, and pollutants on the surface of the target material, such as oil stains, oxide skin and the like, are mainly removed.
(3) The inner and outer surfaces of the qualified engine spray pipe are subjected to oil removal and rust removal, and the coating is mainly cleaned by acid washing and acetone ultrasonic cleaning and is dried to wait for deposition.
(4) The cleaned engine nozzle was placed vertically on the product table, keeping the inner surface of the nozzle on the same center of the circle as the target, while avoiding contact between the target and the product, as shown in fig. 3.
(5) Vacuumizing the vacuum chamber to a vacuum degree of less than or equal to 5 × 10-2At Pa, starting to deposit the coating; the technological parameters are as follows: the arc current is 40-80A, the coil current is 0.2-15A, and the frequency is 1-5 Hz; the deposition time is determined according to the coating thickness requirement, and the thickness of the deposited coating is generally 100-300 μm.
(6) And after the deposition of the coating on the inner surface from the straight line segment of the spray pipe to the throat part is finished, cooling the spray pipe to 45 ℃ along with the vacuum chamber, opening the vacuum chamber and taking out the spray pipe.
(7) The outlet section of the engine nozzle with the deposited coating faces downwards and is vertically placed on a product table, the inner surface of the engine nozzle and the target are kept on the same center of circle, and the target and the product are prevented from contacting with each other, as shown in fig. 4, the engine nozzle is used as a workpiece for depositing the coating and is used as an auxiliary anode; in this example, the distance between the throat and the top end of the molybdenum target is 5mm, and the inner surface coating deposition is performed from the throat to the outlet section of the nozzle.
(8) Vacuum pumping is carried out, when the vacuum degree is less than or equal to 5 multiplied by 10-2At Pa, starting to deposit the coating; the technological parameters are as follows: the arc current is 40-80A, the coil current is 0.2-15A, and the frequency is 1-5 Hz; the deposition time is determined according to the coating thickness requirement, and the thickness of the deposited coating is generally 100-300μm。
(9) And after the inner surface from the outlet section to the throat part is coated with the deposited coating, the engine jet pipe is cooled to 45 ℃ along with the vacuum chamber, and the vacuum chamber is opened to take out the engine jet pipe.
(10) And finishing the deposition of the inner surface coating of the nozzle of the double-component liquid rocket rail attitude control engine.
The invention is described in further detail below with reference to the figures and specific embodiments.
Example 1
As shown in fig. 1, to produce an engine nozzle sized
Figure BDA0001641761200000081
(
Figure BDA0001641761200000082
For example, the minimum inner diameter of the engine nozzle, 100mm for the total length of the engine nozzle), a Mo — W alloy coating is deposited on the inner surface of the engine nozzle.
(a) Preparing an engine spray pipe: machining the engine spray pipe according to the drawing requirements of the engine spray pipe
Figure BDA0001641761200000083
Referring to fig. 1, after the machining, the internal and external surfaces of the engine nozzle are subjected to oil removal and rust removal, and the method mainly comprises the steps of pickling, acetone ultrasonic cleaning and drying, and then waiting for the deposition of a coating.
(b) Preparing a Mo-W alloy coating of the engine spray pipe;
the Mo-W alloy coating is prepared on the inner surface of an engine spray pipe by adopting the following steps:
(1) two Mo-W alloy (Mo: W: 80:20 wt%) cathode targets 1 were machined according to the drawing dimensions, as shown in fig. 2, for a straight-line segment to throat inner surface Mo-W alloy target and a throat to outlet segment inner surface Mo-W alloy target, respectively;
(2) deoiling the Mo-W alloy target used from the straight line section to the inner surface of the throat part, and then installing the Mo-W alloy target on a vacuum cathode arc source device, wherein the vacuum cathode arc source device is used as a cathode;
(3) the straight line segment of the engine spray pipe cleaned in the step (a) faces downwards, and is vertically placed on a product table, the inner surface of the spray pipe and the target are kept on the same center of circle, and the target and the product are prevented from contacting with each other, as shown in figure 3, the engine spray pipe is used as a workpiece for depositing a coating and is used as an auxiliary anode; the distance between the throat part and the top end of the cathode target material is 5 mm.
(4) Vacuum pumping is carried out, and the gauge pressure of the vacuum is less than or equal to 5 multiplied by 10-2Beginning to deposit the Mo-W alloy coating below Pa; deposition process parameters: arc striking voltage: 5000V, arc spot current: 100A, coil current of 0.5-10A and frequency of 2 Hz; the deposition time is 25min, and the thickness of the deposited Mo-W alloy coating is 100-110 μm;
(5) and after the Mo-W alloy coating is deposited on the inner surface from the straight line section to the throat part, cooling the spray pipe to 45 ℃ along with the vacuum chamber, opening the vacuum chamber and taking out the engine spray pipe.
(6) Deoiling the Mo-W alloy target material used on the inner surface from the throat part to the outlet position, and then installing the Mo-W alloy target material on inner surface vacuum cathode arc deposition equipment as a cathode;
(7) the outlet section of the engine nozzle with the deposited Mo-W alloy coating faces downwards and is vertically placed on a product table, the inner surface of the engine nozzle and the target material are kept on the same center of circle, and the target material and the product are prevented from contacting with each other, as shown in FIG. 4, the engine nozzle is used as a workpiece for depositing the coating and is used as an auxiliary anode; in this embodiment, the distance between the throat and the top end of the Mo-W alloy target is 5 mm.
(8) Vacuum pumping is carried out, and the gauge pressure of the vacuum is less than or equal to 5 multiplied by 10-2Beginning to deposit the Mo-W alloy coating below Pa; deposition process parameters: arc striking voltage: 5000V, arc spot current: 120A, coil current of 0.5-15A and frequency of 2-4 Hz; the deposition time is 30min, and the thickness of the deposited Mo-W alloy coating is 110-120 mu m;
(9) and after the Mo-W alloy coating is deposited on the inner surface from the outlet section to the throat part, the engine spray pipe is cooled to 45 ℃ along with the vacuum chamber, and the vacuum chamber is opened to take out the engine spray pipe.
Dissecting and analyzing the spray pipe with the deposited Mo-W coating, and measuring the section thickness and performing microscopic analysis on 1 point of each of the straight line section, the convergent section, the throat section and the outlet section of the spray pipeThe results of the thickness measurements and the microscopic analysis are shown in FIG. 5. from FIG. 5, it can be seen that the inner surface vacuum cathodic arc source achieves an engine nozzle size of
Figure BDA0001641761200000091
The internal surface Mo-W coating deposited, the thickness of the deposited coating: 100-120 μm; coating thickness uniformity: 10 microns, Mo-W coating thickness deposition rate on the inner surface of the nozzle: 4-5 μm/min, and the Mo-W alloy coating is compact.
Example 2
To manufacture an engine nozzle of a size of
Figure BDA0001641761200000092
(
Figure BDA0001641761200000093
200mm for the total length of the engine nozzle) as an example, an iridium coating was deposited on the inner surface of a rhenium nozzle for an engine, illustrating a specific embodiment of the method of the present invention.
(a) Preparing a rhenium spray pipe of an engine: processing the engine spray pipe according to the drawing requirement of the rhenium spray pipe of the engine
Figure BDA0001641761200000101
Referring to fig. 1, after the processing, the internal and external surfaces of the rhenium spray pipe of the engine are subjected to oil removal and rust removal, and the method mainly comprises the steps of pickling, acetone ultrasonic cleaning and drying, and then waiting for the deposition of a coating.
(b) Preparing an iridium coating of a rhenium spray pipe of an engine:
the iridium coating is prepared on the inner surface of the engine spray pipe by adopting the following steps:
(1) machining a profiling iridium (99.98 at.%) cathode inner target (as shown in figure 2) according to the drawing size, wherein the profiling iridium inner target is an iridium target for the inner surface from a straight line section to a throat part and an iridium target for the inner surface from the throat part to an outlet section;
(2) after the iridium target material used from the straight line section to the inner surface of the throat part is deoiled, the iridium target material is installed on inner surface vacuum cathode arc deposition equipment to be used as a cathode;
(3) the straight line segment of the engine spray pipe cleaned in the step (a) faces downwards, and is vertically placed on a product table, the inner surface of the spray pipe and the target are kept on the same center of circle, and the target and the product are prevented from contacting with each other, as shown in figure 3, the engine spray pipe is used as a workpiece for depositing a coating and is used as an auxiliary anode; in this example, the distance between the throat and the tip of the molybdenum target was 8 mm.
(4) Vacuum pumping is carried out, and the gauge pressure of the vacuum is less than or equal to 5 multiplied by 10-2Beginning to deposit the iridium coating below Pa; deposition process parameters: arc striking voltage: 5000V, arc spot current: 60A, coil current of 0.5-15A and frequency of 3 Hz; the deposition time is 40min, and the thickness of the deposited iridium coating is 200-210 μm;
(5) and after the deposition of the iridium coating on the inner surface from the straight line segment to the throat part is finished, cooling the spray pipe to 45 ℃ along with the vacuum chamber, opening the vacuum chamber and taking out the engine spray pipe.
(6) After the iridium target material used on the inner surface from the throat part to the outlet position is degreased, the iridium target material is installed on inner surface vacuum cathode arc deposition equipment to be used as a cathode;
(7) the outlet section of the engine spray pipe with the deposited iridium coating faces downwards and is vertically placed on a product table, the inner surface of the spray pipe and the target are kept on the same center of circle, and the target and the product are prevented from contacting with each other, as shown in figure 4, the engine spray pipe is used as a workpiece for depositing the iridium coating and is used as an auxiliary anode; in this embodiment, the distance between the throat and the top end of the iridium target is 5 mm.
(8) Vacuum pumping is carried out, and the gauge pressure of the vacuum is less than or equal to 5 multiplied by 10-2Beginning to deposit the iridium coating below Pa; deposition process parameters: arc striking voltage: 5000V, arc spot current: 60A, coil current of 0.5-15A and frequency of 3 Hz; the deposition time is 60min, and the thickness of the deposited Mo-W alloy coating is 280-300 mu m;
(9) after the deposition of the iridium coating on the inner surface from the outlet section to the throat part is finished, the engine jet pipe is cooled to 45 ℃ along with the vacuum chamber, and the vacuum chamber is opened to take out the engine jet pipe.
Dissecting and analyzing the spray pipe with deposited iridium coating, taking 1 point from each of the straight line section, the convergent section, the throat section and the outlet section of the spray pipe to perform section thickness measurement and microscopic analysis, wherein the results of the thickness measurement and the microscopic analysis are shown in FIG. 6As can be seen in fig. 6, the experiment shows: the size of the engine spray pipe is realized by the inner surface vacuum cathode arc source
Figure BDA0001641761200000111
The internal surface iridium coating deposited, the thickness of the deposited coating: 280-300 μm; coating thickness uniformity: 10 microns, deposition rate of iridium coating thickness on the inner surface of the nozzle: 4.8-5 μm/min, and the iridium coating is continuous and compact.
The above description is only for the best mode of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Those skilled in the art will appreciate that the invention may be practiced without these specific details.

Claims (8)

1. A vacuum cathode arc source device is characterized in that: the device comprises a cathode target (1), a non-magnetic stainless steel auxiliary anode (2), a non-contact high-voltage pulse arc striking (3), a cooling water pipe (4), a mandrel (5) and an electromagnetic coil (6);
the electromagnetic coil (6) is wound outside the mandrel (5), one end of the mandrel (5) is connected with the cathode, the other end of the mandrel (5) is connected with the cylindrical section at the bottom end of the cathode target (1) through threads, and the cooling water pipe (4) penetrates through the mandrel (5) and then extends to the conical section at the top end of the cathode target (1); the non-magnetic stainless steel auxiliary anode (2) is sleeved on the outer surface of the cylindrical section of the cathode target (1); the non-contact high-voltage pulse arc ignition (3) is fixedly connected with the non-magnetic stainless steel auxiliary anode (2) through a threaded through hole on the side surface of the non-magnetic stainless steel auxiliary anode (2);
when the inner diameter of the spray pipe is more than 20mm, the cathode target (1) comprises a hollow cylindrical section and a hollow conical section; the top end of the conical section is an arc transition section which is matched with the convergence section of the spray pipe; the conical section is positioned above the cylindrical section, and the included angle between the generatrix of the conical section and the central axis of the conical section is 8-13 degrees; the inner surface of the cylindrical section is provided with internal threads, the height of the cylindrical section is 8-10mm, the height of the conical section is h, the length from the nozzle opening to the throat is L, h is L-d, and d is 5-8;
when the inner diameter of the spray pipe is less than or equal to 20mm, the cathode target (1) comprises a hollow cylindrical section, a transition section and a hollow conical section, the transition section is positioned between the cylindrical section and the hollow conical section, the top end of the conical section is an arc transition section, and the arc transition section is matched with the convergence section of the spray pipe; the conical section is positioned above the transition section, the transition section is positioned above the cylindrical section, and an included angle between a generatrix of the conical section and a central axis of the conical section is 8-13 degrees; the inner surface of the cylindrical section is provided with internal threads, the height of the cylindrical section is 8-10mm, the height of the conical section is h, the length from the nozzle opening to the throat is L, h is L-d, and d is 5-8; the height of the transition section is 20-25 mm.
2. A vacuum cathodic arc source apparatus as defined in claim 1 wherein: the distance between the end surface of the copper core of the non-contact high-voltage pulse arc ignition (3) and the outer surface of the cylindrical section of the cathode target (1) is 1-2 mm;
the cathode target (1) is made of iridium, rhenium, niobium, molybdenum, Mo-W, Nb-W, Hf-Ta or MCrAlYSiB.
3. A vacuum cathodic arc source apparatus as defined in claim 1 wherein: the nonmagnetic stainless steel auxiliary anode (2) is a hollow cylinder, the inner diameter of the hollow cylinder is 10-15mm larger than the maximum outer diameter of the cathode target (1), and the outer diameter of the hollow cylinder is 50-60 mm; the height of the hollow cylinder is consistent with that of the cylinder section of the cathode target (1); the side surface of the non-magnetic stainless steel auxiliary anode (2) is provided with a threaded through hole.
4. A vacuum cathodic arc source apparatus as defined in claim 1 wherein: the non-contact high-voltage pulse arc striking (3) comprises a copper core, a ceramic sleeve and a molybdenum sleeve, wherein the ceramic sleeve is sleeved outside the copper core, the molybdenum sleeve is sleeved outside the ceramic sleeve, the diameter of the copper core is 2-3mm, the length of the copper core is 10-20mm larger than that of the ceramic sleeve, the inner diameter of the ceramic sleeve is matched with that of the copper core, the length of the ceramic sleeve is 30-35mm, the outer diameter of the ceramic sleeve is 10-12mm, the inner diameter of the molybdenum sleeve is matched with that of the ceramic sleeve, the length of the molybdenum sleeve is 10-15mm smaller than that of the ceramic sleeve, and the wall thickness of the molybdenum sleeve is 1-3 mm; the outer surface of the molybdenum sleeve is provided with external threads.
5. A vacuum cathodic arc source apparatus as defined in claim 1 wherein: the material of the mandrel (5) is a magnetic conductive material with low remanence; the mandrel (5) is a hollow cylinder, the outer surface of the top end of the mandrel (5) is provided with external threads, and the wall thickness of the mandrel (5) is 3-5 mm; the outer diameter of the mandrel (5) is 20-25 mm.
6. A vacuum cathodic arc source apparatus as defined in claim 1 wherein: the electromagnetic coil (6) is made of high-temperature-resistant enameled copper wire wound, the number of winding turns is 500-800 turns, the height is 100-150mm, and the inner diameter of the electromagnetic coil (6) is matched with the outer diameter of the mandrel (5).
7. A method for depositing a coating on an interior surface of a rocket motor nozzle utilizing a vacuum cathodic arc source apparatus as recited in any one of claims 1-6, characterized in that the method comprises the steps of:
(1) placing a cathode target (1), a non-magnetic stainless steel auxiliary anode (2) and a non-contact high-voltage pulse arc striking (3) in a vacuum cathode arc source device into a vacuum chamber, wherein an electromagnetic coil (6) is positioned outside the vacuum chamber, one part of a cooling water pipe (4) and a mandrel (5) is positioned in the vacuum chamber, and the other part of the cooling water pipe (4) and the mandrel (5) is positioned outside the vacuum chamber;
(2) cleaning the inner surface of the spray pipe and drying;
(3) sleeving the spray pipe cleaned in the step (2) on the outer surface of the cathode target (1) in the step (1), and vacuumizing a vacuum chamber; the spray pipe is coaxial with the cathode target (1), and the inner surface of the spray pipe is not contacted with the cathode target (1); the conical sections of the cathode target (1) are all positioned in the spray pipe;
(4) when the vacuum degree is less than 5 multiplied by 10-2Pa, using arc depositionDepositing a coating on the inner surface of the nozzle;
(5) and after the deposition of the coating is finished, cooling for more than 3 hours under the vacuum condition, and then taking out the spray pipe to obtain the spray pipe with the coating deposited on the inner surface.
8. A method of depositing a coating on an internal surface of a rocket motor nozzle as recited in claim 7, wherein: in the step (4), the arc deposition process parameters are as follows: the current of the electromagnetic coil (6) is direct current, triangular waves are adopted for the current, the amplitude is 0.2-15A, the frequency of the current is 1-5Hz, the distance and the height of the arc spot moving on the surface of the cathode target material (1) are realized by adjusting the amplitude of the current, and the speed of the arc spot moving up and down on the surface of the cathode target material (1) is controlled by controlling the frequency of the current; the arc current of the arc deposition is 40-80A; the thickness of the deposited coating is 100-300 μm.
CN201810384095.XA 2018-04-26 2018-04-26 Vacuum cathode arc source device and coating deposition method Active CN108588650B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810384095.XA CN108588650B (en) 2018-04-26 2018-04-26 Vacuum cathode arc source device and coating deposition method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810384095.XA CN108588650B (en) 2018-04-26 2018-04-26 Vacuum cathode arc source device and coating deposition method

Publications (2)

Publication Number Publication Date
CN108588650A CN108588650A (en) 2018-09-28
CN108588650B true CN108588650B (en) 2020-04-10

Family

ID=63609577

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810384095.XA Active CN108588650B (en) 2018-04-26 2018-04-26 Vacuum cathode arc source device and coating deposition method

Country Status (1)

Country Link
CN (1) CN108588650B (en)

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU528386A1 (en) * 1975-07-07 1976-09-15 Предприятие П/Я В-8495 Sorption Vacuum Pump
RU2099573C1 (en) * 1995-04-27 1997-12-20 Исследовательский центр им.М.В.Келдыша Electric arc rocket engine
AT413953B (en) * 2003-11-25 2006-07-15 Fronius Int Gmbh METHOD AND CIRCUIT FOR TOUCH-FREE IGNITION OF A WELDING ARC
US7444955B2 (en) * 2004-05-19 2008-11-04 Sub-One Technology, Inc. Apparatus for directing plasma flow to coat internal passageways
US7790003B2 (en) * 2004-10-12 2010-09-07 Southwest Research Institute Method for magnetron sputter deposition
CN204281846U (en) * 2014-12-05 2015-04-22 大连维钛克科技股份有限公司 A kind of novel magnetic field structure of vacuum ion membrane plating equipment
CN105112857B (en) * 2015-07-24 2017-08-25 航天材料及工艺研究所 A kind of motor power chamber body portion prepares the method that iridium and silicide combine coating
CN204825032U (en) * 2015-07-28 2015-12-02 东莞市汇成真空科技有限公司 Arc spot that discharges is abound with vacuum cathode arc source of target surface
CN106001554B (en) * 2016-06-29 2018-06-01 航天材料及工艺研究所 A kind of preparation method of rhenium iridium combustion chamber

Also Published As

Publication number Publication date
CN108588650A (en) 2018-09-28

Similar Documents

Publication Publication Date Title
US10272468B2 (en) Integrated fluidjet system for stripping, prepping and coating a part
US10752994B2 (en) Apparatus and method for depositing a coating on a substrate at atmospheric pressure
CN107227445B (en) A kind of arc ion plating apparatus of deposited tube inside coating
US7867366B1 (en) Coaxial plasma arc vapor deposition apparatus and method
KR910009164B1 (en) Zirconium nitride coated article and method for making same
US8038858B1 (en) Coaxial plasma arc vapor deposition apparatus and method
CN105779925B (en) The method that supersonic flame spraying fore-put powder carries out laser melting coating
CN102758186B (en) Electric arc ion plating apparatus
US4904528A (en) Coated gas turbine engine compressor components
CN104108054B (en) Large complicated metal surface plasma body and pulsed discharge composite polishing processing device
CN100460555C (en) Equipment and method for low temperature depositing high-quality decorative film by electric arc ion plating
CN108588650B (en) Vacuum cathode arc source device and coating deposition method
CN111155082A (en) Preparation method of FeCoNiCrMn high-entropy alloy coating
Le et al. Studying the microhardness on the surface of SKD61 in PMEDM using tungsten carbide powder
CN110158056A (en) Vacuum coater
CN113862618B (en) Blade of aircraft engine and preparation method thereof
CN105112872A (en) Pulse magnetron sputtering device for preparing inner surface coating of cylinder part and application of pulse magnetron sputtering device
CN112921293A (en) High-silicon molybdenum silicide composite gradient coating on inner and outer surfaces of engine thrust chamber body and preparation method thereof
JP2014051699A (en) Apparatus for forming alloy thin film
RU2362838C2 (en) Device for nano-cluster plating
JP4502116B2 (en) High density plasma surface coating method and apparatus
JP6573276B2 (en) Thin film generator using magnetized coaxial plasma generator
US20150101924A1 (en) Assembly and method of coating an interior surface of an object
CN113385672B (en) Processing device and method for composite coating on inner surface of pipe fitting
Vasylyev et al. DEPOSITION OF THE DIAMOND-LIKE COATINGS ON THE SURFACES OF THE RING-SHAPED DRY GASEOUS SEALS MADE OF SiC FORUSE IN HIGH PRESSURE COMPRESSORS

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant