CN101575696B - Preparation method of chromium-aluminum-nitrogen film by closed field unbalanced magnetron sputtering - Google Patents
Preparation method of chromium-aluminum-nitrogen film by closed field unbalanced magnetron sputtering Download PDFInfo
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- CN101575696B CN101575696B CN2009100747790A CN200910074779A CN101575696B CN 101575696 B CN101575696 B CN 101575696B CN 2009100747790 A CN2009100747790 A CN 2009100747790A CN 200910074779 A CN200910074779 A CN 200910074779A CN 101575696 B CN101575696 B CN 101575696B
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Abstract
The invention relates to a preparation method of a chromium-aluminum-nitrogen film by closed field unbalanced magnetron sputtering, which comprises the following steps: a chromium-tungsten-manganese steel plate is taken as a basal body, chromium and aluminum as a target source of metal ion, nitrogen gas as reactant gas, and argon gas as ion bombardment gas and protection gas; in a vacuum sputtering furnace, in a closed magnetic field state, in the argon gas and at the temperature of 300 DEG C, the surface of the chromium-tungsten-manganese steel plate is sputtered with chromium ion, aluminum ion and nitrogen ion and the chromium-aluminum-nitrogen hard film is formed on the surface of the steel plate, and then the low temperature tempering and alloying solid solution are conducted, thus greatly improving mechanical property, hardness, intensity, abrasive resistance and erosion resistance of the surface of the chromium-tungsten-manganese steel plate. The mechanical property of the chromium-tungsten-manganese steel plate can be improved by 466% compared with that of hardened steel plates. The preparation method has short process flow, precise technique, accurate and detailed measurement values, the film with thickness of 4,600nm, and the alloy layer with good solid solution effect and being not easy to peel off, thus being the ideal treatment method for strengthening and hardeningthe surface of alloy tool steel.
Description
Technical field
The present invention relates to the method that a kind of closed field unbalanced magnetron sputtering prepares chromium-aluminum-nitrogen film, belong to the technical field of high-strength, high hardness material surface coating and application.
Background technology
In the machine building industry field, using a large amount of metallic substance, because it is purposes is different with requirement, also different to the processing of material, the worker who for example has high strength, high rigidity touches tool and wear-resistant, corrosion resistant mechanical component, all needs it is strengthened, increases hard processing.
To the enhancing of instrument, mould and mechanical component, increase hard processing, several different methods is also arranged, for example surface alloying infiltrates elements such as nickel, chromium, molybdenum, silicon, to strengthen its intensity, hardness at metal material surface; Heat treating process for example at high temperature changes the inside metallographic structure of metal, to improve hardness, the intensity of material, also has the metallic cementation method, high-frequency quenching method etc.
Ganoine thin film is one of effective way of improving workpiece surface wear resistance and resistance to high temperature oxidation, film deposition techniques mainly comprises chemical vapour deposition and physical vapor deposition, chemical vapour deposition is because the depositing temperature height, its application on matrix is restricted, physical vapor deposition is because depositing temperature is low, applicable base material range is wide, and film quality is easy to control, has obtained widespread use; Physical vapor deposition mainly comprises vacuum evaporation and sputtering sedimentation, film densification, film-substrate cohesion that sputtering method generates are good, use wider, the sputter coating mode has radio-frequency sputtering, triode sputtering and magnetron sputtering, magnetron sputtering other sputters relatively has higher plated film speed, magnetron sputtering develops into non-equilibrium magnetic controlled from initial conventional magnetic control, unbalanced magnetron, at present, non-equilibrium magnetic controlledly combine with the multi-source closed magnetic field, the plasma density of vacuum chamber is improved, the ion bombardment effect strengthens, and can obtain better quality of coating; Adopt the closed field unbalanced magnetron sputtering plated film, owing to sputtering condition, target source material, metal difference, the sputter coating effect also has many difference and deficiency, also has a lot of drawbacks, and for example thicknesses of layers is balanced inadequately, technical parameter instability etc.
Summary of the invention
Goal of the invention
Purpose of the present invention is exactly at disadvantages of background technology, adopts the closed field unbalanced magnetron sputtering method, carries out sputter coating on chromium tungsten manganese steel material surface, generates chromium aluminium nitrogen ganoine thin film, to increase substantially hardness, intensity and the wear resistance on chromium tungsten manganese steel surface.
Technical scheme
The chemical substance material that the present invention uses is: chromium tungsten manganese steel plate, acetone, nitrogen, argon gas, chromium piece, aluminium block, deionized water, lapping powder, its combination consumption is as follows: with gram, milliliter, centimetre
3Be measure unit
Chromium tungsten manganese steel plate: 1 of Cr WMn 200 * 100 * 20mm
Chromium piece: 2 of Cr 720 * 120 * 6mm
Aluminium block: 2 of Al 720 * 120 * 6mm
Acetone: CH
3COCH 10000ml ± 100ml
Nitrogen: N
2100000cm
3± 100cm
3
Argon gas: Ar 100000cm
3± 100cm
3
Deionized water: H
2O 10000ml ± 100ml
Lapping powder: 600 in aluminum oxide
The closed field unbalanced magnetron sputtering legal system is equipped with chromium aluminium nitrogen ganoine thin film:
(1) selected material, chemical substance
To carry out selectedly to preparing required chemical substance material, and carry out shape, size, precision, quality purity control:
Chromium tungsten manganese steel plate: the solid-state solid of CrWMn, contain Cr 1.03%, W 1.3%, and Mn 0.92%, Si0.29%, C 1.09%
Chromium piece: solid-state solid, 99.99%
Aluminium block: solid-state solid, 99.99%
Acetone: liquid liquid, 99.9%
Deionized water: liquid liquid, 99.6%
Nitrogen: gaseous state gas, 99.99%
Argon gas: gaseous state gas, 99.99%
Lapping powder: particle diameter is even
(2) mechanical slicing chromium tungsten manganese steel plate
With six of the slicings on mechanical Bao bed of the chromium tungsten manganese steel plate of 200 * 100 * 20mm, each face is vertical, surface roughness Ra 2.5-5 μ m;
(3) chromium tungsten manganese steel plate thermal treatment
1. quench hot: chromium tungsten manganese steel plate is placed the high-temperature heat treatment stove, carry out quench hot, quenching temperature is 870 ℃, and surface hardness HRC63-65, heat-eliminating medium are machine oil;
2. low-temperaturetempering places tempering stove with the chromium tungsten manganese steel plate after quenching, and tempering temperature is 200 ℃, tempering insulation time 120min;
(4) mechanical grinding chromium tungsten manganese steel plate
With quench hot and six of mechanical planarization grinding machines of tempered chromium tungsten manganese steel plate, each face is vertical, surface roughness Ra 0.08-1.6 μ m;
(5) grind chromium tungsten manganese steel plate
With the chromium tungsten manganese steel plate after the grinding, grind chromium tungsten manganese steel plate working-surface, surface roughness Ra 0.02-0.04 μ m with 600 lapping powder;
(6) ultrasonic cleaning chromium tungsten manganese steel plate, chromium is fast, aluminium is fast
Chromium tungsten manganese steel plate after grinding is placed ultrasonic cleaner, add acetone 2000ml, ultrasonic cleaning 20min uses washed with de-ionized water then, dries, and puts into vacuum chamber, and is standby;
Two chromium pieces are placed ultrasonic cleaner, add acetone 2000ml, ultrasonic cleaning 20min uses washed with de-ionized water then, dries, and puts into vacuum chamber, and is standby;
Two aluminium blocks are placed ultrasonic cleaner, add acetone 2000ml, ultrasonic cleaning 20min uses washed with de-ionized water then, dries, and puts into vacuum chamber, and is standby;
(7) clean the magnetron sputtering stove
1. open the magnetron sputtering stove,, make its cleaning with dirt and dust in the suction cleaner suction furnace chamber;
2. scrub the magnetron sputtering furnace chamber with deionized water, make its cleaning;
3. clean magnetron sputtering stove fire door, bell, sealing cover with acetone, make its cleaning;
(8) place sputtering source
1. the chromium piece with two 720 * 120 * 6mm places on the interior symmetrical sputtering target platform of sputter furnace chamber, and fixing;
2. the aluminium block with two 720 * 120 * 6mm places on the interior symmetrical sputtering target platform of sputter furnace chamber, and fixing;
3. ion source is placed on the symmetrically arranged ion source(-)holder, and fixing;
(9) place chromium tungsten manganese steel plate
Grinding, cleaning, dried chromium tungsten manganese steel plate are vertically placed the rotary work-table sidepiece in the magnetron sputtering furnace chamber, and fixing;
(10) place chromium piece, aluminium block
Chromium piece after cleaning, aluminium block intersected be symmetrically placed on chromium target stand in the furnace chamber, the aluminium target stand;
(11) preparation chromium aluminium nitrogen ganoine thin film in the vacuum magnetic-control sputtering stove
1. close sputter stove sealing cover;
2. open the water cycle condensing works of sputter stove outside, make the sputter stove be in condensing state;
3. open vacuum pump, vacuumize in the furnace chamber, make the interior vacuum tightness of furnace chamber reach 6 * 10
-3Pa;
4. open sputter stove well heater, heating chromium tungsten manganese steel plate, temperature rises to 300 ℃ ± 5 ℃ by 20 ℃, and constant temperature, insulation;
5. import argon gas, carry out the argon gas ion bombardment: open tunger tube, argon bottle, in furnace chamber, import argon gas, input speed 280cm
3/ min makes the interior pressure values of furnace chamber continue to remain on 2Pa;
6. open two chromium targets, volts DS 400V, power 4.4kW, chromium target 10min is cleaned in the argon gas ion bombardment, removes chromium target oxide on surface;
7. open two aluminium targets, volts DS 370V, power 3.4kW, argon ion bombardment clean aluminium target 10min, remove aluminium target oxide on surface;
8. open rotary work-table, the uniform rotation of chromium tungsten manganese steel plate, velocity of rotation 3r/min;
9. open two ion sources, volts DS 230V, power 1.2kW, argon gas is with 280cm
3The flow velocity of/min the ion source of flowing through produces plasma body after the ionization, plasma bombardment surface of steel plate 30min removes oxide on surface;
10. continue applying argon gas, make the interior vacuum tightness of stove remain on 2.4 * 10
-1Pa starts ion source and chromium target simultaneously, and ion source volts DS 110V, power are 1.2kW, chromium target volts DS 360V, power 2.4kW, and at surface of steel plate deposition chromium layer, time 5min, the steel plate bias voltage is-300V;
Open the aluminium target, aluminium target volts DS 370V, power 3.4kW deposit chromium layer, aluminium lamination simultaneously at surface of steel plate, time 5min, and the steel plate bias voltage is-300V;
Sputter stove well heater is closed in cooling, makes the chromium tungsten manganese steel plate of sputter chromium-aluminum-nitrogen film cool to 20 ℃ ± 3 ℃ with the furnace;
(12) chromium tungsten manganese steel plate is taken out in blow-on
Close argon bottle, open bell, take out chromium tungsten manganese steel plate, place clean environment;
(13) low-temperaturetempering, alloying solid solution, cooling
The chromium tungsten manganese steel plate that 1. will be coated with the chromium-aluminum-nitrogen film layer places the tempering heat treatment stove, and low-temperaturetempering is handled under argon shield, 150 ℃ ± 5 ℃ of tempering temperatures, tempering time 60min, argon gas input speed 200cm
3/ min forms the alloying solid solution layer after the tempering;
2. the tempering stove well heater is closed in cooling after the tempering, under argon shield, cools to 20 ℃ ± 3 ℃ with the furnace;
(14) blow-on
Take out the chromium tungsten manganese steel plate after the tempering, that is: be coated with the chromium tungsten manganese steel plate of chromium-aluminum-nitrogen film layer;
(15) detect, chemically examine, analyze, characterize, contrast
Pattern, color and luster, composition, mechanical property and the metallurgical structure on the chromium tungsten manganese steel plate surface that is coated with the chromium-aluminum-nitrogen film layer to preparation detects, chemically examines, analyzes, characterizes, contrasts;
Analyze chromium tungsten manganese steel plate and film transverse section and surface topography with the JSM-6700F field emission scanning electron microscope;
Measure the knoop hardness HK of film with MH-5 type microhardness tester;
With M03XHF22 type X-ray diffractometer the chromium-aluminum-nitrogen film structure is analyzed;
(16) storage package
The chromium tungsten manganese steel plate that is coated with chromium-aluminum-nitrogen film to preparation is packed with soft material, places cool place, drying, clean environment, waterproof, protection against the tide, acid-proof alkali salt to corrode 20 ℃ ± 3 ℃ of storing temps, relative humidity≤10%.
Describedly be equipped with chromium aluminium nitrogen ganoine thin film with the closed field unbalanced magnetron sputtering legal system, in the vacuum magnetic-control sputtering stove, carry out, its preparation state is: in the bottom of sputter body of heater 1 is stove seat 2, is sealing cover 3 on the top of sputter body of heater 1, and the inside of sputter body of heater 1 is furnace chamber 27; Left part at sputter body of heater 1 is provided with argon bottle 9, and argon bottle 9 connects with the argon gas mouth 22 of sputter stove upper left quarter by argon gas valve 10, tunger tube 11, and with furnace chamber 27 UNICOMs; The right part of sputter body of heater 1 is provided with nitrogengas cylinder 12, and nitrogengas cylinder 12 is by nitrogen valve 13, nitrogen tube 14 and the nitrogen mouth 23 of sputter body of heater 1 upper right quarter, ion source 15,16 UNICOMs in the furnace chamber 27; Right part at nitrogengas cylinder 12 is provided with vacuum pump 6, and vacuum pump 6 is by vacuum valve 7, valve tube 8 and furnace chamber 27 UNICOMs; The mid-way is provided with rotary work-table 4 in furnace chamber 27, and rotary work-table 4 inside are well heater 26, and rotary work-table 4 sidepieces are chromium tungsten manganese steel plate 5 fixedly; Symmetrical spaced set chromium target 17,19, aluminium target 18,20, ion source 15,16 on the furnace wall in furnace chamber 27; Liquid crystal display 28, cabinet switch 24, pilot lamp 25 are set on housing 2; It in furnace chamber 27 nitrogen+argon gas mixed gas 21; In the outside of sputter body of heater 1 is water cycle condensing works 35; On ion source 15,16, be provided with electro-magnet 29,30, on chromium target 17,19, be provided with electro-magnet 31,32, on aluminium target 18,20, be provided with electro-magnet 33,34.
The chromium-aluminum-nitrogen film of described closed field unbalanced magnetron sputtering method preparation, thickness is 4600nm, its film hardness is 33.6GPa.
The chromium-aluminum-nitrogen film of described closed field unbalanced magnetron sputtering method preparation; be to be matrix with chromium tungsten manganese steel plate; with chromium piece and aluminium block is splash-proofing sputtering metal target source, is reactant gases with nitrogen, is ion bombardment gas and shielding gas with the argon gas, finishes under 300 ℃ ± 5 ℃ states of heating.
Described preparation chromium-aluminum-nitrogen film, chromium target volts DS 360V, power 2.4kW, aluminium target volts DS 370V, power 3.4kW, ion source volts DS 110V, power are 1.2kW.
Beneficial effect
The present invention compares with background technology has tangible advance, it is to be matrix with chromium tungsten manganese steel plate, with the chromium piece, aluminium block is the sputtering target source, with nitrogen is reactant gases, in the vacuum sputtering stove, keeping substrate temperature is 300 ℃, under non-equilibrium closed magnetic field state, in argon gas atmosphere, form chromium-aluminum-nitrogen film on chromium tungsten manganese steel plate surface, carry out low-temperaturetempering then, the alloying solid solution, form alloying layer after making chromium tungsten manganese steel plate surface and the solid solution of chromium-aluminum-nitrogen film layer, make the mechanical property on chromium tungsten manganese steel plate surface, hardness, intensity, wear resistance, erosion resistance is greatly improved, can improve 466% than the steel plate mechanical property of hardening, this preparation method's technical process is short, technology is tight, value is accurate, and the alloy layer solid solution is effective, difficult drop-off is the enhancing of very good chromium tungsten manganese alloy tool steel surface, increase hard method.
Description of drawings
Fig. 1 prepares the state graph of chromium aluminium nitrogen ganoine thin film for the magnetron sputtering stove
Fig. 2 is chromium tungsten manganese steel plate, chromium target, aluminium target, an ion source layout drawing in the sputter stove
Fig. 3 is sputter stove preparation temperature and time coordinate graph of a relation
Fig. 4 is a chromium aluminium nitrogen ganoine thin film square section shape appearance figure
Fig. 5 is a chromium aluminium nitrogen ganoine thin film surface topography map
Fig. 6 is a chromium aluminium nitrogen ganoine thin film diffracting surface intensity collection of illustrative plates
Shown in the figure, list of numerals is as follows:
1, the sputter body of heater, 2, the stove seat, 3, sealing cover, 4, rotary work-table, 5, chromium tungsten manganese steel plate, 6, vacuum pump, 7, vacuum valve, 8, valve tube, 9, argon bottle, 10, the argon gas valve, 11, tunger tube, 12, nitrogengas cylinder, 13, nitrogen valve, 14, nitrogen tube, 15, ion source, 16, ion source, 17, the chromium target, 18, the aluminium target, 19 chromium targets,, 20, the aluminium target, 21, argon gas+nitrogen mixture body, 22, the argon gas mouth, 23, the nitrogen mouth, 24, cabinet switch, 25, pilot lamp, 26, well heater, 27, sputtering chamber, 28, liquid crystal display, 29, electro-magnet, 30, electro-magnet, 31, electro-magnet, 32, electro-magnet, 33, electro-magnet, 34, electro-magnet, 35, the water cycle condensing works.
Embodiment:
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, for the magnetron sputtering stove prepares the state graph of chromium aluminium nitrogen ganoine thin film, it is correct that want each position, installs firmly, easy for operation.
Argon bottle, nitrogengas cylinder, vacuum pump will rationally be prepared, pressure values is constant in the furnace chamber during plated film, gas is sufficient, chromium target, aluminium target symmetry equidistantly are arranged on the furnace wall, under closed Nonequilibrium magnetic field action, make argon ion quicken the bombardment target, make chromium, aluminium atomic deposition to substrate, form chromium aluminium nitrogen ganoine thin film with the nitrogen ionization, each parameter value, temperature are controlled automatically by computer program.
Material, the value that uses in this preparation is to determine by the scope that sets in advance, with gram, milliliter, centimetre
3Be measure unit.
In chromium target, aluminium target, the ion source electro-magnet is housed all, the magnetic line of force intensity of electro-magnet is adjusted variation according to the sputter needs, makes magnetic field be in nonequilibrium situations, and magnetic line of force intensity is regulated and control in 150-400 tesla.
Preparation is to carry out under the clean state of strictness, and under closed field unbalanced magnetic control state, in argon gas atmosphere, has prevented the intervention of objectionable impurities element, has guaranteed severity, the accuracy of test.
The closed field unbalanced magnetron sputtering principle of work:
In the closed field unbalanced magnetron sputtering, strengthen or weaken for the opposite polar magnetic field of another polarity by polar magnetic field of target source magnetron, form non-equilibrium distributed magnetic field, adjacent between the magnetron simultaneously with opposite pole, magnetic line of force each other interconnects, form the magnetic line of force loop line, electronics is carried out the most effective constraint, the density of vacuum chamber is improved; In vacuum chamber, ar atmo is ionized out a large amount of argon ions and electronics under electric field action, and electronics flies to chromium tungsten manganese steel plate, and argon ion quickens the bombardment target under electric field action, sputter a large amount of target atom, is the neutral target atom and is deposited on film forming on the substrate; In addition, secondary electron is influenced by non-equilibrium closed magnetic field Lip river logical sequence magnetic force in quickening to fly to the process of substrate, be bound in the plasma body zone of target surface, plasma density height in this zone, secondary electron in moving process constantly bump ionization go out a large amount of argon ions and remove to bombard target, reduce gradually through the energy of electronics after the collision repeatedly, break away from the magnetic line of force constraint, away from target, finally be deposited on the substrate.
Inventive principle:
Closed field unbalanced magnetron sputtering deposition chromium-aluminum-nitrogen film, adopt Metal Cr and Al to make sputtering target material, when increasing negative bias, also increased gas ion source to matrix, make reactant gases nitrogen directly feed the ion source target body, even gas distribution and ionization are carried out in the slit by giving vent to anger, under the effect of ion source power electrical field, a large amount of the GN 2 ions obtain kinetic energy and fly to workpiece surface, argon ion quickens bombardment a large amount of target atom that target sputtered and also is deposited on surface of steel plate under electric field action simultaneously, chromium element and nitrogen element interaction form face-centred cubic chromium nitride in the plasma environment of closed field unbalanced magnetron sputtering system, aluminium element is solidly soluted in the chromium nitride lattice and forms chromium-aluminum-nitrogen film simultaneously, and chromium-aluminum-nitrogen film mainly is made up of three parts: the Cr bottom of 0.2 μ m, 0.4 the Cr+Al of μ m ladder coating, the CrAlN composite bed of 4 μ m; Metal Cr bottoming stage and Al, Cr composition alternation stage provide enough bonding strength and hardness to support to film top layer respectively in the thin film growth process, and at the growth phase of film top layer CrAlN layer, along with the hardness of the increase film of nitrogen content also improves thereupon.
Shown in Figure 2, be chromium tungsten manganese steel plate, chromium target, aluminium target, ion source layout drawing in the sputter furnace chamber, chromium target, aluminium target, ion source are intersection dislocation symmetric arrangement, are beneficial to evenly obtain when chromium tungsten manganese steel plate rotates on rotational plane coating; Chromium tungsten manganese steel plate vertically is installed on the rotary work-table, and working face is outside, is beneficial to aim at each target source when worktable rotates, and the rotary work-table revolution must not be too fast, is advisable with 3r/min.
Shown in Figure 3, be sputter stove preparation temperature and time coordinate graph of a relation, among the figure as can be known: temperature begins to heat up by 20 ℃, i.e. the A point, speed with 10 ℃/min rises to 300 ℃ ± 5 ℃, and promptly the B point prepares in this temperature sputter, the constant temperature insulation, be the B-C section, cool to 20 ℃ then with the furnace, be i.e. the D point.
Shown in Figure 4, for chromium aluminium nitrogen ganoine thin film square section shape appearance figure, can find out obviously between chromium-aluminum-nitrogen film and the matrix surface among the figure to form transition layer that transition layer and film and matrix bond are tight, solid solubility is good.
Shown in Figure 5, be chromium aluminium nitrogen ganoine thin film surface topography map, among the figure as can be known: the membrane structure densification, crystal grain is tiny evenly, the film macrobead is to be assembled by many small-particles to form.
Shown in Figure 6, be chromium aluminium nitrogen ganoine thin film diffracted intensity collection of illustrative plates, among the figure as can be known: ordinate zou is that diffracted intensity, X-coordinate are diffraction angle 2 θ, at 2 θ is the diffraction peak that there are AlN (100) at 33.1 degree places, is respectively 37.54,43.73 and 63.54 diffraction peaks of CrN (111), CrN (200) and CrN (220) respectively when spending at 2 θ.
Claims (5)
1. a closed field unbalanced magnetron sputtering prepares the method for chromium-aluminum-nitrogen film, it is characterized in that: the chemical substance material of use is: chromium tungsten manganese steel plate, acetone, nitrogen, argon gas, chromium piece, aluminium block, deionized water, lapping powder, its combination consumption is as follows: with gram, milliliter, centimetre
3Be measure unit
Chromium tungsten manganese steel plate: 1 of Cr WMn 200 * 100 * 20mm
Chromium piece: 2 of Cr 720 * 120 * 6mm
Aluminium block: 2 of Al 720 * 120 * 6mm
Acetone: CH
3COCH
310000ml ± 100ml
Nitrogen: N
2100000cm
3± 100cm
3
Argon gas: Ar 100000cm
3± 100cm
3
Deionized water: H
2O 10000ml ± 100ml
Lapping powder: 600 in aluminum oxide
The closed field unbalanced magnetron sputtering legal system is equipped with chromium-aluminum-nitrogen film:
(1) selected material, chemical substance
To carry out selectedly to preparing required chemical substance material, and carry out shape, size, precision, quality purity control:
Chromium tungsten manganese steel plate: the solid-state solid of CrWMn, contain Cr 1.03%, W 1.3%, and Mn 0.92%, Si0.29%, C 1.09%
Chromium piece: solid-state solid, 99.99%
Aluminium block: solid-state solid, 99.99%
Acetone: liquid liquid, 99.9%
Deionized water: liquid liquid, 99.6%
Nitrogen: gaseous state gas, 99.99%
Argon gas: gaseous state gas, 99.99%
Lapping powder: particle diameter is even
(2) mechanical slicing chromium tungsten manganese steel plate
With six of the slicings on mechanical Bao bed of the chromium tungsten manganese steel plate of 200 * 100 * 20mm, each face is vertical, surface roughness Ra 2.5-5 μ m;
(3) chromium tungsten manganese steel plate thermal treatment
1. quench hot: chromium tungsten manganese steel plate is placed the high-temperature heat treatment stove, carry out quench hot, quenching temperature is 870 ℃, and surface hardness HRC63-65, heat-eliminating medium are machine oil;
2. low-temperaturetempering places tempering stove with the chromium tungsten manganese steel plate after quenching, and tempering temperature is 200 ℃, tempering insulation time 120min;
(4) mechanical grinding chromium tungsten manganese steel plate
With quench hot and six of mechanical planarization grinding machines of tempered chromium tungsten manganese steel plate, each face is vertical, surface roughness Ra 0.08-1.6 μ m;
(5) grind chromium tungsten manganese steel plate
With the chromium tungsten manganese steel plate after the grinding, grind chromium tungsten manganese steel plate working-surface, surface roughness Ra 0.02-0.04 μ m with 600 lapping powder;
(6) ultrasonic cleaning chromium tungsten manganese steel plate, chromium piece, aluminium block
Chromium tungsten manganese steel plate after grinding is placed ultrasonic cleaner, add acetone 2000ml, ultrasonic cleaning 20min uses washed with de-ionized water then, dries, and puts into vacuum chamber, and is standby;
Two chromium pieces are placed ultrasonic cleaner, add acetone 2000ml, ultrasonic cleaning 20min uses washed with de-ionized water then, dries, and puts into vacuum chamber, and is standby;
Two aluminium blocks are placed ultrasonic cleaner, add acetone 2000ml, ultrasonic cleaning 20min uses washed with de-ionized water then, dries, and puts into vacuum chamber, and is standby;
(7) clean the magnetron sputtering stove
1. open the magnetron sputtering stove,, make its cleaning with dirt and dust in the suction cleaner suction furnace chamber;
2. scrub the magnetron sputtering furnace chamber with deionized water, make its cleaning;
3. clean magnetron sputtering stove fire door, bell, sealing cover with acetone, make its cleaning;
(8) place sputtering source
1. the chromium piece with two 720 * 120 * 6mm places on the interior symmetrical sputtering target platform of sputter furnace chamber, and fixing;
2. the aluminium block with two 720 * 120 * 6mm places on the interior symmetrical sputtering target platform of sputter furnace chamber, and fixing;
3. ion source is placed on the symmetrically arranged ion source(-)holder, and fixing;
(9) place chromium tungsten manganese steel plate
Grinding, cleaning, dried chromium tungsten manganese steel plate are vertically placed the rotary work-table sidepiece in the magnetron sputtering furnace chamber, and fixing;
(10) place chromium piece, aluminium block
With chromium piece, the aluminium block after cleaning, intersection is symmetrically placed on the interior chromium target stand of furnace chamber, the aluminium target stand;
(11) preparation chromium aluminium nitrogen ganoine thin film in the vacuum magnetic-control sputtering stove
1. close sputter stove sealing cover;
2. open the water cycle condensing works of sputter stove outside, make the sputter stove be in condensing state;
3. open vacuum pump, vacuumize in the furnace chamber, make the interior vacuum tightness of furnace chamber reach 6 * 10
-3Pa;
4. open sputter stove well heater, heating chromium tungsten manganese steel plate, temperature rises to 300 ℃ ± 5 ℃ by 20 ℃, and constant temperature, insulation;
5. import argon gas, carry out the argon gas ion bombardment: open tunger tube, argon bottle, in furnace chamber, charge into argon gas, input speed 280cm
3/ min makes the interior pressure values of furnace chamber continue to remain on 2Pa;
6. open two chromium targets, volts DS 400V, power 4.4kW, chromium target 10min is cleaned in the argon gas ion bombardment, removes chromium target oxide on surface;
7. open two aluminium targets, volts DS 370V, power 3.4kW, argon ion bombardment clean aluminium target 10min, remove aluminium target oxide on surface;
8. open rotary work-table, the uniform rotation of chromium tungsten manganese steel plate, velocity of rotation 3r/min;
9. open two ion sources, volts DS 230V, power are 1.2kW, and argon gas is with 280cm
3The flow velocity of/min the ion source of flowing through produces plasma body after the ionization, plasma bombardment surface of steel plate 30min removes oxide on surface;
10. continue applying argon gas, make the interior vacuum tightness of stove remain on 2.4 * 10
-1Pa starts ion source and chromium target simultaneously, and ion source volts DS 110V, power are 1.2kW, chromium target volts DS 360V, power 2.4kW, and at surface of steel plate deposition chromium layer, time 5min, the steel plate bias voltage is-300V;
Sputter stove well heater is closed in cooling, makes the chromium tungsten manganese steel plate of sputter chromium-aluminum-nitrogen film be chilled to 20 ℃ ± 3 ℃ with stove;
(12) chromium tungsten manganese steel plate is taken out in blow-on
Close argon bottle, open bell, take out chromium tungsten manganese steel plate, place clean environment;
(13) low-temperaturetempering, alloying solid solution, cooling
The chromium tungsten manganese steel plate that 1. will be coated with the chromium-aluminum-nitrogen film layer places the tempering heat treatment stove, and low-temperaturetempering is handled under argon shield, 150 ℃ ± 5 ℃ of tempering temperatures, tempering time 60min, argon gas input speed 200cm
3/ min forms the alloying solid solution layer after the tempering;
2. the tempering stove well heater is closed in cooling after the tempering, cools to 20 ℃ ± 3 ℃ under argon shield with the furnace;
(14) blow-on
Take out the chromium tungsten manganese steel plate after the tempering, that is: be coated with the chromium tungsten manganese steel plate of chromium-aluminum-nitrogen film;
(15) detect, chemically examine, analyze, characterize, contrast
Pattern, color and luster, composition, mechanical property and the metallurgical structure on the chromium tungsten manganese steel plate surface that is coated with chromium-aluminum-nitrogen film to preparation detects, chemically examines, analyzes, characterizes, contrasts;
Analyze chromium tungsten manganese steel plate and film transverse section and surface topography with the JSM-6700F field emission scanning electron microscope;
Measure the knoop hardness HK of film with MH-5 type microhardness tester;
With M03XHF22 type X-ray diffractometer the chromium-aluminum-nitrogen film structure is analyzed;
(16) storage package
The chromium tungsten manganese steel plate that is coated with chromium-aluminum-nitrogen film to preparation is packed with soft material, places cool place, drying, clean environment, waterproof, protection against the tide, acid-proof alkali salt to corrode 20 ℃ ± 3 ℃ of storing temps, relative humidity≤10%.
2. a kind of closed field unbalanced magnetron sputtering according to claim 1 prepares the method for chromium-aluminum-nitrogen film, it is characterized in that: describedly be equipped with chromium-aluminum-nitrogen film with the closed field unbalanced magnetron sputtering legal system, in the vacuum magnetic-control sputtering stove, carry out, its preparation state is: in the bottom of sputter body of heater (1) is stove seat (2), on the top of sputter body of heater (1) is sealing cover (3), and the inside of sputter body of heater (1) is furnace chamber (27); Left part at sputter body of heater (1) is provided with argon bottle (9), and argon bottle (9) connects with the argon gas mouth (22) of sputter stove upper left quarter by argon gas valve (10), tunger tube (11), and with furnace chamber (27) UNICOM; The right part of sputter body of heater (1) is provided with nitrogengas cylinder (12), and nitrogengas cylinder (12) is by nitrogen valve (13), nitrogen tube (14) and the nitrogen mouth (23) of sputter body of heater (1) upper right quarter, ion source (15, the 16) UNICOM in the furnace chamber (27); Right part at nitrogengas cylinder (12) is provided with vacuum pump (6), and vacuum pump (6) is by vacuum valve (7), valve tube (8) and furnace chamber (27) UNICOM; The mid-way is provided with rotary work-table (4) in furnace chamber (27), and rotary work-table (4) inside is well heater (26), and rotary work-table (4) sidepiece is chromium tungsten manganese steel plate (5) fixedly; Symmetrical spaced set chromium target (17,19), aluminium target (18,20), ion source (15,16) on the furnace wall in furnace chamber (27); Liquid crystal display (28), cabinet switch (24), pilot lamp (25) are set on housing (2); It in furnace chamber (27) nitrogen+argon gas mixed gas (21); In the outside of sputter body of heater (1) is water cycle condensing works (35); On ion source (15,16), be provided with electro-magnet (29,30), on chromium target (17,19), be provided with electro-magnet (31,32), on aluminium target (18,20), be provided with electro-magnet (33,34).
3. a kind of closed field unbalanced magnetron sputtering according to claim 1 prepares the method for chromium-aluminum-nitrogen film, it is characterized in that: described chromium-aluminum-nitrogen film with the preparation of closed field unbalanced magnetron sputtering method, thickness is 4600nm, and its film hardness is 33.6GPa.
4. a kind of closed field unbalanced magnetron sputtering according to claim 1 prepares the method for chromium-aluminum-nitrogen film; it is characterized in that: described closed field unbalanced magnetron sputtering legal system is equipped with chromium-aluminum-nitrogen film; be to be matrix with chromium tungsten manganese steel plate; with chromium piece and aluminium block is splash-proofing sputtering metal target source; with nitrogen is reactant gases; with the argon gas is ion bombardment gas and shielding gas, finishes under 300 ℃ ± 5 ℃ states of heating.
5. a kind of closed field unbalanced magnetron sputtering according to claim 1 prepares the method for chromium-aluminum-nitrogen film, and its chromium aluminium nitrogen thicknesses of layers is 4600nm, and wherein chromium layer 200nm, chromium+aluminium gradient layer 400nm, chromium+aluminium+nitrogen composite bed are 4000nm.
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| CN102345606A (en) * | 2011-10-19 | 2012-02-08 | 上海西工压缩机配件有限公司 | GCr15 compressor blade subjected to surface modification and manufacture process thereof |
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