CN1097221A - The method and apparatus of metal material surface alloying - Google Patents
The method and apparatus of metal material surface alloying Download PDFInfo
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- CN1097221A CN1097221A CN 93107796 CN93107796A CN1097221A CN 1097221 A CN1097221 A CN 1097221A CN 93107796 CN93107796 CN 93107796 CN 93107796 A CN93107796 A CN 93107796A CN 1097221 A CN1097221 A CN 1097221A
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- metallic cementation
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- gas generator
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Abstract
A kind of by metal and metallic compound steam by the method and apparatus of metallic cementation material surface metallic cementation.Be placed on the very aerial negative electrode by the metallic cementation material, feed and desire the metallic cementation halide vapor, be provided with the work producer in the vacuum chamber and make the desire metallic cementation flash to steam.High-pressure electricity between negative electrode and anode and produce glow discharge.What be positioned at negative electrode is infiltrated the metal of desiring to ooze by the metallic cementation material under the effect of glow discharge.
Description
The present invention relates to a kind of method and apparatus of metal material surface alloying, a kind of more precisely method and apparatus that utilizes the reaction product steam of work gas generator in halogenide atmosphere of desiring the making of metallic cementation material to carry out ion implantation as the alloying element source.
The method of ion implantation is extremely paid attention in industrial broad prospect of application because of it.This method is to other metallic cementations, and following advantage is arranged: the surface alloy infiltration layer combines firmly with body material, and energy consumption is lower, and the alloying element consumption is few, and labor condition is good etc., and its application has remarkable economic efficiency and social benefit.From present case, this method is to have very big development potentiality, in numerous reports, significant following two kinds of situations are arranged:
(1) with the gas mixture of metal halide gas and other gas such as hydrogen etc. or with the ion implantation method of single metal halide gas (latter such as Chinese patent CN85107593) as the glow discharge work atmosphere, its advantage is to realize that the device structure of this method is simpler, and special processing parameter is few etc.About 600 ℃, nickel, iron etc. is oozed Al, get final product to such an extent that be respectively AlNi, AiNi to the top layer
3, NiAl
3And Fe
3Al, Fe
2Al
5, FeAl
3Deng the metal layer, iron, nickel are oozed titanium respectively then can obtain this method respectively and obtain FeTi, Ni
3Ti or the like alloy layer.But these class methods are owing to only used halide gas as the metallic cementation source, and the concentration that contains infiltration element in its work gas is lower, has caused the efficient of metallic cementation also lower.
(2) double-layer metallic glow ion cementation (U.S. Pat 4520268) and arc discharge ion implantation (Chinese patent CN88100549.5).The characteristics of these class methods are to carry out direct heating to desiring metallic cementation, the steam that ion bombardment or arc discharge make it to evaporate is as work gas, emphasis point is to provide desires the higher work gas of metallic cementation concentration of element as the metallic cementation source, in the hope of improving the efficient of metallic cementation.Its main drawback is a direct heating, the chemically reactive of the source metallics that ion bombardment and arc discharge are evaporated is not so good as last class methods, and because of its on than source metal boiling point to much lower temperature under the degrees of freedom of particle motion very limited, be difficult to be full of equably reaction compartment with it as work gas.As the former, source electrode have only with wait to ooze part from nearer (as 50～100mm) time, effect has just significantly influenced the quality of metallic cementation greatly.Source electrode needs bigger surface-area and very high temperature in addition, also makes equipment complicated.
The objective of the invention is to collect the advantage of above each method, overcome shortcoming wherein, proposed a kind of novel solution, so that the efficient of metallic cementation improves greatly, infiltration layer contains gold element content height, and is firm with matrix bond, and is evenly distributed.
Specifically, main points of the present invention are indoor except that conventional negative electrode, anode are set at vacuum reaction, have also set up the work gas generator that consumes as the metallic cementation source.This work gas generator is 13.3Pa-1.33 * 10 at pressure
3Keep a kind of reactive mode in the halogenide atmosphere that is easy to get of Pa, hollow cathode discharge, and with the atmosphere of work gas generator and halide reaction generation as work atmosphere.Because the work gas generator is made with desiring the metallic cementation material, to be subjected to violent chemical reaction when the corresponding work state is kept in energising in desiring metallic cementation halogenide atmosphere and generate more at a low price halogenide, the halogenide of these new generations flashes to gas under the high temperature in a vacuum and replaces former halide gas gradually and be full of reaction chamber and become work atmosphere.Because the metallic element atomic percent has improved in the halogenide at a low price, thereby make that the concentration of infiltration element greatly improves in the work atmosphere, on the other hand, halogenide generally has lower boiling point, thereby its steam particle freedom of motion journey is more much bigger than the free path of simple metal vapors particle under working temperature, is full of space, entire reaction chamber and homogenizing easily.Consider from the chemically reactive aspect that again owing to be in ionized state by the most of particle in the atmosphere of work gas generator generation, add the existence of the high halogens of chemically reactive, work gas can keep very high chemically reactive.Like this and anode and waiting ooze between the negative electrode of material and add high direct voltage and produce glow discharge, be incubated as required, can obtain required alloy layer.
Fig. 1 is a kind of equipment synoptic diagram of realizing aforesaid method, realizes the process of aforesaid method below in conjunction with this schematic view illustrating.
Vacuum reaction chamber (1) vacuumizes through pumped vacuum systems (2), metal material for seep (3) places on the negative electrode (4), at indoor work gas generator (5) and the anode (6) of also being provided with in addition of vacuum reaction, halide vapor source (7) connects with vacuum reaction chamber, AC transformation power supply (8) can give preheating furnace (9) power supply of heating in the vacuum chamber to the vacuum reaction chamber preheating as the case may be, barometer (10) is measured air pressure in the vacuum chamber, when vacuumize make vacuum reach more than the 13.3Pa after, the halide vapor in halide vapor source (7) is filled with indoor the making of vacuum reaction and reaches 13.3-13.3 * 10 in it3The operating pressure of Pa, the power supply (11) of connection work gas generator (5) makes work gas generator (5) keep normal work; Connect glow discharge dc source (22), produce glow discharge between negative electrode (4) and anode (6), the negative pressure on the negative electrode (4) keeps 500-1200 ℃ for the treatment of temperature between 400-1200V, processing time just can obtain infiltration layer in workpiece (3) generally more than 10 minutes.
In said process, work gas generator (5) is the hollow cathode device of making by wanting metallic cementation. And can place simultaneously two or more work gas generators according to size and the workpiece distribution situation of reative cell.
In the said process, can determine as the case may be whether preheating oven (9) and power supply (8) thereof use.For example, in the time of need toasting body of heater and workpiece etc. and the higher and glow discharge energy of treatment temp can not keep this temperature the time, promptly enable preheating oven; And when not needing baking and subzero treatment, then preheating oven can.
Also need detection and monitoring instrument, instrument, thermopair and the temperature instrumentation (14) of some necessity in the said process, put into the valve (13) of air etc., some component can be implemented water-cooled (as furnace shell, electrode etc.).
Embodiment one: the carbon steel sample oozes titanium, the work gas generator is the hollow cathode discharge device, makes of industrially pure titanium.Halide vapor is titanium tetrachloride (TiCl
4) steam.Process is as follows, and carbon steel work-piece (3) places on the negative electrode (4), and vacuum system (2) vacuumizes; But variable-voltage power supply (8) electricity makes preheating oven (9) to vacuum reaction chamber (1) preheating, its voltage 50-200V, preheating temperature 600-900 ℃; Reach 13.3Pa when above with vacuum tightness, charge into TiCl
4Gas makes the operating pressure that reaches 13.3-1.33hPa in it; Connect power supply (11) and just keep works better to hollow cathode discharge work gas generator (5).Connect glow discharge power supply (12) between negative electrode and anode, voltage remains on 400-1200V, keeps the glow discharge of sample, and to make treatment temp be 700-1200 ℃, and insulation is more than 10 minutes.Respectively to 10
#, 20
#, 45
#, T8, T10 steel etc. ooze titanium respectively.Found that, be lower than 0.2% carbon steel for carbon content, only formed the titanium carbide (TiC) of part in its surface, this is the result that small amount of carbon combines with the titanium that infiltrates to the top layer diffusion in the sample, but because of carbon content is lower, thus can not form successive TiC film, and for carbon content greater than 0.3% carbon steel, the surface of sample has then formed the pure TiC film of bright and clean densification, has the performance of high rigidity and good antiacid, caustic corrosion.The X-ray diffraction spectrum of T8 steel after oozing titanium is TiC.
Embodiment two: the carbon steel sample oozes nickel.The work gas generator is the hollow cathode device, and makes of pure nickel, and the work gas of feeding is NiCl
2, all the other similar process.After the processing, can obtain the surface of iron-nickel alloy.
Other embodiment: molybdenum system work gas generator (hollow cathode or feeding MoCl
5Gas.Then form carbide such as the MoC of Mo at steel surface
2And Fe
3Mo
2, α phase, γ equate the Fe-Mo alloy layer of composition.Titanium system work gas generator, logical TiCl
4, contain Ni in the formation of Ni base alloy surface
3Ti, NiTi
2Alloy layer, form at Cu base alloy surface and to contain CuTi
2, Cu
3Ti and Cu
4The alloy layer of Ti.W makes the work gas generator, logical WCl
2Steam then forms by Fe at steel surface
7W
6, Fe
2W
2C, WC, W
2The infiltration layer that C and αGu Rongti are formed.With the work producer that graphite is made, logical CCl
4Gas then forms carbon metallizing thing.
Claims (9)
1, a kind of with the steam of desiring metallic cementation and its halide reaction products therefrom as the glow discharge of the gas of working in the method for the treatment of metallic cementation material surface metallic cementation, be made up of following process: vacuum reaction chamber vacuumizes and makes its vacuum tightness more than 13.3pa; Charge into the halide vapor of desiring metallic cementation, make it to reach 13.3Pa-1.33 * 10
3The operating pressure of Pa; Connection be in the vacuum chamber by the power supply of desiring the work metal vapors producer that metallic cementation makes, make it under above-mentioned operating pressure, to react with above-mentioned halide vapor, and its temperature is raise, the product of reaction is thereupon evaporating in a vacuum and replacing former halide vapor gradually and become work gas; Waiting to ooze the high direct voltage that adds a 400-1200V between the work negative electrode of material and anode in placement makes it keep glow discharge; Keep treatment temp 500-1200 ℃ as required with more than the treatment time 10min, wait to ooze the material surface alloying, it is characterized in that thereby make:
Above-mentioned work gas generator is the hollow cathode discharge device.
2, according to claim 1,2 method, the power supply that it is characterized in that the work producer is a direct supply, and voltage is 200-800V.
3, according to the method for right 1,2, air pressure 13.3-13.3 * 10 when it is characterized in that generation hollow cathode discharge that work takes place
3Pa.
4, according to the method for right 1,3, the gas that it is characterized in that producing hollow cathode discharge is halogenide.
5, a kind of equipment that passes through the compound steam glow discharge metallic cementation of desire metallic cementation, comprising: a vacuum reaction chamber and pumped vacuum systems thereof; Place a sun inspection of vacuum reaction chamber, a negative electrode that is electrically connected with part to be oozed and one or more work gas generator; One be connected with vacuum reaction chamber wait to ooze the element halide vapor source; Two covers are respectively negative electrode and the work gas generator provides the power supply of voltage; Above-mentioned work gas generator is the hollow cathode discharge device.
6,, it is characterized in that described vacuum reaction chamber has a cover primary heater unit according to equipment in method in the right 1 and the right 5.
7,, it is characterized in that described work gas generator is to desire the metallic cementation material to make according to the equipment in the right 5.
8, according to the equipment of right 5, the power supply of work producer is independently.
9, according to right 6, the power supply of primary heater unit is alternating-current or direct current in the vacuum reaction chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93107796 CN1097221A (en) | 1993-07-08 | 1993-07-08 | The method and apparatus of metal material surface alloying |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93107796 CN1097221A (en) | 1993-07-08 | 1993-07-08 | The method and apparatus of metal material surface alloying |
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| CN1097221A true CN1097221A (en) | 1995-01-11 |
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ID=4986859
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|---|---|---|---|
| CN 93107796 Pending CN1097221A (en) | 1993-07-08 | 1993-07-08 | The method and apparatus of metal material surface alloying |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010060259A1 (en) * | 2008-11-03 | 2010-06-03 | 北京坚润表面材料研究所 | Preparation of atomizing gas, method and equipment of forming novel material by atomizing gas discharging |
-
1993
- 1993-07-08 CN CN 93107796 patent/CN1097221A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010060259A1 (en) * | 2008-11-03 | 2010-06-03 | 北京坚润表面材料研究所 | Preparation of atomizing gas, method and equipment of forming novel material by atomizing gas discharging |
| US8795770B2 (en) | 2008-11-03 | 2014-08-05 | Beijing Tough & Lubricating Institute | Preparation of mist, process and apparatus for forming new materials by mist gas discharge |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |