DD202456A5 - PROCESS FOR MELTING - Google Patents

Abstract

A method for fusing a second conductive member to the matrix of a first conductive member is provided wherein the second member is brought into contact with the first conductive member in either a solid or dissociable solution and a chopped electrical signal certain frequency is suspended.

Description

Iz lengthwise process

Field of application of the invention

Lie invention "relates to fusion processes, plants for carrying out such processes and products from such processes,

This application is a partial follow-up to US Pat. No. 224,762, filed January 13, 1981.

For the purposes of this application, the term "fusion" is intended to mean a process by which various elements are chemically or physically linked.

Characteristic of the known technical solutions;

So far, it has been common practice to treat substrates or matrices in a variety of ways to improve the characteristics of the matrix for a particular application. Sometimes the matrix was treated as a body in these treatments, and in other techniques only the surface characteristics were increased »

However, these techniques had limitations. The workpiece or matrix may have a certain shape which is not suitable for carrying out a specific process increasing the characteristic values; the process may destroy already present desired properties of the workpiece; or the treated workpiece, although having certain improved characteristics, may have other reduced properties.

In general, the method used depends on the workpiece to be treated or the matrix to be treated and the desired properties.

More specifically, coating techniques, heat treatment, anodization, arc spraying, vacuum evaporation, chemical deposition, sputtering and ion plating are all common processes,

Non-ferrous metals can be hardened by aging, heat treatment or anodizing »

231151.1982 * 024536

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By α iese. However, techniques do not provide adequate protection against dry abrasion wear.

By. Spray coating techniques could not improve the corrosion resistance or physical properties of ferrous materials.

The abrasion resistance of non-ice substrate could be improved by electrochemical or electromechanical plating with hard chrome, but this measure is expensive and time consuming. "

The other techniques, such as arc spraying, vacuum evaporation and sputtering, also have disadvantages because the applied layer is usually thin, interfacial bonding strength is poor, or it can only be used to treat small surface areas. "

In practical use, the disadvantages are that guest techniques or high voltages are required, which cause difficulties and limit their versatility.

For ease of reference, in this specification ^{, the} term "first conductive chemical element" shall refer to the matrix with which the fusion is to occur, and the term "chemical element" shall denote such element or an alloy thereof; "second conductive chemical element or an alloy thereof" is intended to indicate the item that is to be merged with the _matrix.:

It is also intended that the term "fusion" as used in this specification should be understood as meaning penetration of atoms or molecules of a second element into the solid matrix of a first element or alloy thereof.

Aim of the invention;

The invention is therefore based on the object, at least partially eliminate these disadvantages by a novel method and a system for merging the various

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most conductive elements are provided with either iron-containing or light-iron matrices.

It is another object of the invention to provide a novel apparatus and method utilizing a deposition technique at ambient temperatures that achieves high bond strength without distortion or loss of workpiece or die memory properties.

Another object of the invention relates to a method in which the use of process gas-air is not required and in which no security risks occur and are caused by the no "heat distortion.

Yet another object of the invention relates to a process which requires a low energy input and the coating material is nevertheless used effectively.

Another object of the invention is to provide a plant that is cheap and portable so easy.

Yet another object of the invention relates to a method by which a solid interfacial bonding is provided, and which does not require skilled workers for execution.

It is another object of the invention to provide solutions of conductive chemical elements which can be used for the fusion of these chemical elements with solid matrices of other conductive elements or alloys thereof.

It is also an object of the invention to produce new and improved products which will have improved physical and chemical properties.

Explanation of the essence of the invention:

According to the invention, there is provided a method, apparatus and solutions for altering the surface properties of a metal or alloy thereof at ambient temperatures by physically applying a second conductive chemical element to the substrate

L · w U / \ U L

Surface whose characteristics are to be changed, and that applying a chopped electrical signal of a certain frequency to both elements when in physical contact are used,

Ea a plant is created, which has a resonant circuit for generating a half-wave signal at the output and means for the connection of a second element to be melted, and the first chemical element, with which the second is to be fused, with the output.

Solutions are also provided for use in the process and in connection with the plant. These solutions consist of a solution of a conductive chemical of the chemical to be melted in a dissociable form; which may be present in an amount of from 0.10 to 10 masses and has a pH ranging from 0.4 to 14. Ea is favorable if the specific. Resistance of the. Solution in the range of 5 to 500 ohm-cm, preferably between 10 and 80 ohm-cm,

Was melted by the 'application of the procedure for ^1-ferrous and ilicht-Eisenmatrizen new products are generated, in which a second "chemisches- conductive element in a first chemical' conductive element to a depth of more than 0.5 / tun and a surface layer of the second chemical conductive element has been applied in thicknesses greater than 0.5 / μm.

! Ausführungsbe games;

These and other objects and features of the invention will become more apparent from the following description and drawings, in which specific embodiments of the process plant and of products of the method for illustrating the invention are explained.

In the drawings:

Fig. 1 is a general perspective view of an embodiment of the fiction, according to the system ', which is used for the inventive method-j

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FIG. 2 is a general perspective view of a second embodiment of the installation according to the invention, which is used for the method according to the invention; FIG.

Fig. 3 is a schematic electrical circuit for the invention;

Fig. 4 is a circuit diagram of an oscillator used for installation in an embodiment of the invention;

Fig. 5 is a photomicrograph at 500x magnification of a steel sample treated with titanium mococarbide according to the invention; , ,

Fig. 6 is a photomicrograph at 110x magnification showing the penetration of titanium into the treated specimen of Fig. 5;

Fig. 7 is a photomicrograph scan with an electron scanning microanalyser (EPMA) of the Ti-K surface layer of the test specimen, the section of which is shown in Figs. 5 and 6;

Fig. 8 is a photomicrograph at 1100 magnification of the specimen shown in Fig. 5 after heavy hickel plating and polishing to show the thickness of the deposit;

Figs. 9 to 16 are EPMA line scans respectively of locations 1 to 8 as indicated in Fig. 5;

Figure 17 is an EPMA scan of the Ti-enriched zone marked in Figure 8;

Fig. 18 is a composite micrograph taken with a scanning microscope (SEM) having right and left halves, a steel matrix to which molybdenum has been fused by a solid molybdenum electrode by the method of the present invention; the left half is a 655x magnification and the right half is a 1965x magnification of the area marked in the left half;

18A is a composite micrograph, with right and left half, another steel matrix, with the molybdenum using the method according to the invention of a solid Mo-

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molybdenum electrode fused-became; the left half is a 1310-fold magnification and the right half a 3930-fold magnification of the area marked in the left half;

Pig. Fig. 19 is a diagram of a SM / EPIvIA of the sample shown in Fig. 18, showing the fusion of molybdenum with the steel;

Fig. 19A is a diagram of a scanning microscopic scan of the sample shown in Fig. 19, showing the fusion of molybdenum with the steel;

20 shows a SH.I micrograph at 1310 × magnification of a steel matrix with which tungsten has been fused by a solid tungsten electrode by means of the method according to the invention;

Fig. 21 is a diagram of an SEM / EPMA scan of the sample shown in Fig. 20, showing the fusion of tungsten with the steel;

Fig. 22 is a composite SEM micrograph, with right and left halves, of a copper matrix fused to molybdenum from a molybdenum solution using the method of the present invention. The left half is a 1250x magnification.- and the "right" half is an 8x magnification of the area marked in the left half;

Fig. 23 is a diagram of an SEM / EPMA scan of the sample shown in Fig. 22, showing the fusion of molybdenum with copper;

Figure 24 is a composite SEM micrograph, right and left half, of a steel matrix to which molybdenum was fused from a molybdenum solution using the method of the present invention. The left half is a 1250x magnification and the right half is an 8x magnification of the area marked in the left half;

Fig. 25 is a diagram of an SEM / EPMA scan of the sample shown in Fig. 24, showing the fusion of molybdenum with steel;

Fig. 26 is a composite micrograph, with right and left half, a copper matrix, with the tungsten using the

Yerfahrena invention was fused from a tungsten solution. The left half is a 1250x magnification and the right half is an 8x magnification of the area marked in the left half;

FIG. 27 shows a further SSI micrograph of the sample of FIG. 26 at a magnification of 10,000 times a portion of the region marked in FIG. 26; FIG.

28 is a diagram of a SEM / ΕΡΜΑ scanning of the sample shown in Figures 2 and ¹ S 2ψ £ P)..;

FIG. 29 is a composite micrograph, with right and left halfs, of a steel matrix to which tungsten has been fused from a tungsten solution using the method of the present invention ^; left half is a 1310x magnification and the right half is an 8x magnification of the area marked in the left half;

Fig. 30 is a diagram of an SM / SPMA scan of the sample shown in Fig. 29, showing the fusion of tungsten with steel;

31 shows a composite micrograph, with right and left halves, of a copper matrix, with which indium was fused with the aid of the method according to the invention from an indium solution. The left half is a 1250x magnification and the right half "is an 8x magnification of the area marked in the left half;

Fig. 32 is a diagram of an electron microprobe scan of the sample shown in Fig. 31;

33 shows a composite SM micrograph, with right and left halves, of a steel matrix to which indium has been fused from an indium solution using the method according to the invention. The left half is a 625x magnification and the right half is 8x the area marked in the left half;

Fig. 34 'is a diagram of an SEM / SPMA scan of the sample shown in Fig. 33;

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Fig. 35 is a cross-section SEM micrograph, with right and left halves, of a copper matrix fused to nickel from a nickel package using the method of the present invention. The left half is a 1250X magnification and the right half is an 8X magnification. magnify dea in the left half marked area;

Fig. 36 is a diagram of an SM / EPMA scan of the sample shown in Fig. 35;

Fig. 37 is a composite SEM micrograph with right and left halves, a steel matrix, fused with nickel from the nickel solution using the process of the present invention, the left half is a 1310x magnification, and the right half is one 8x magnification of the area marked in the left half;

Fig. 38 is a diagram of an SEM / EPMA scan of the sample shown in Fig. 37; '

Fig. 39 is a composite micrograph of a copper matrix with which gold has been fused. The. left half is a 1310x magnification and the right half is an 8x magnification of the area marked in the left half;

Fig. 40 is a diagram of an SEM / SPMA scan of the sample shown in Fig. 39 showing fused gold ⁽ kJ) with the copper matrix;

Fig. 41 is a composite micrograph, with right and left halves, of a steel matrix to which gold has been fused using the process of the present invention. The left half is a 1310x magnification and the right half is an 8x magnification of the area marked in the left half;

Fig. 42 is a diagram of an SM / EPMA scan of the sample shown in Fig. 40, showing gold molten in the steel matrix;

FIG. 43 shows an SEM micrograph magnified 10 000 times from a copper matrix with which chromium is deposited using the

In accordance with the invention, the process was melted from a first chromium solution.

Pig. FIG. 44 is a diagram of an SM / SPM A scan of the sample shown in FIG. 43 showing the fusion of chromium with copper 5. FIG

Fig. 45 shows an SEM micrograph magnified 10,000X from a steel matrix to which chromium has been fused using the method of the present invention from the above-mentioned first chromium solution;

Fig. 46 is a diagram of an SEM / EPMA scan of the sample shown in Fig. 45, showing the fusion of chromium with steel;

47 shows a composite SEM micrograph, with right and left half, of a copper matrix, with which chromium was fused from a second chromium solution using the method according to the invention. The left half is a 625x magnification and the right half is an 8x magnification of the area marked in the left half;

Fig. 47A is a more enlarged SEEvI-M ikr ο at the enlarged portion of Fig. 47 at a magnification of 10,000X;

Fig. 48 is a diagram of an SEM / EPMA scan of the sample shown in Fig. 47, showing the fusion of chromium with copper;

49 shows a composite SEM micrograph, with right and left half, of a steel matris with which chromium has been fused from a second chromium solution using the method according to the invention. The left half is a 1250x magnification and the right half is an 8x magnification • of the area marked in the left half;

Fig. 49A shows a more enlarged SM-axis at the magnified area of Fig. 49 at a magnification of 10,000X;

Fig. 50 is a diagram of an SM / EPMA scan of the sample shown in Fig. 48 showing the fusion of chromium with steel;

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Pig. 51 a composite micrograph, with right and left halves, of a copper matrix with which cadmium has been fused from a first cadmium solution using the invented method; the left half is a 1310x magnification and the right half is a 5x magnification of the marked area;

Fig. 52 is a diagram of an SEM / EPMA scan of the type shown in Flg. 51, which shows a fusion of cadmium with copper;

Fig. 53 is a micrograph at 11 500 x magnification ... of a steel matrix to which cadmium has been fused using the "cadmium" second solution of the present invention;

Fig. 54 is a diagram of an SM / EPMA scan of the sample shown in Fig. 53, showing the fusion of cadmium with steel;

Figure 55 is a composite micrograph, with right and left halves, of a copper matrix, with which tin has been fused from a first tin solution using the method of the present invention; the., left half is a 655x magnification and the right half is an 8x magnification of the marked area;

Fig. 55 shows an SEM / EPMA scan of the sample of Fig. 55 showing the fusion of tin with pluck; shows;

Figure 57 is a composite micrograph, with right and left halves, of a copper matrix to which tin has been fused using the process of the present invention from a second tin solution; the left half is a 326x magnification and the right half is an 8x magnification of the marked area;

Fig. 58 is an SEM / EPMA scan of the sample of Fig. 57 showing the fusion of tin with copper; ,

Figure 59 is a composite SEM micrograph, with right and left half of a steel matrix, with the tin using the

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inventive method was fumigated from the second tin solution; the right half is a 1310x magnification and the left half is an 8x magnification of the marked area;

Fig. 60 shows an SEM / EPMA scan of the type in Pig. 59, which shows the fusion of tin with steel;

Pig. Figure 61 shows an SEM micrograph at 5200 magnification of a copper matrix to which cobalt has been fused from a first cobalt solution using the method of the present invention; -

Pig. Fig. 62 is an SEM / EPMA scan of the sample shown in Fig. 61 showing the fusion of cobalt with copper;

FIGS. 63 and 63A are micrographs of a copper matrix fused to silver from a first silver solution using the method of the invention;

Fig. 63 is a composite wherein the left half is 625 times magnification and the right half is 8 times magnification of the marked area.

Fig. 63A is a more magnified SM micrograph of the enlarged portion of Fig. 63 at 10,000X magnification;

Fig. 64 is an SEM / EPMA scan of the sample of Fig. 63 showing the fusion of silver with copper;

Fig. 65 shows an SEM micrograph magnified 10,000X from a copper matrix to which silver has been fused from a second silver solution using the method of the present invention;

FIG. 66 shows an electron microprobe scan of the sample of FIG.

65, which shows the fusion of silver with copper *

In the diagrams; illustrative figures, from Fig. 19 to Figo

66, the vertical axis is logarithmic, while the horizontal axis is linear. And in these diagrams, the surface layer was determined at the point where the concentration (ingot) of the matrix and the fused therewith

- • 12 -

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Both elements are both 50 % , as illustrated by the extensions. V

The pig. 1 and 2 of the drawings show a general perspective view of the installation according to the invention, which is used to carry out the method according to the invention »

In Pig. 1, which illustrates a solid-solid process, the number 10 designates an energy source and 11 an oscillator «

One side of the oscillator output is connected by a socket 12 to the electrode 13. The socket 12 is provided with a rotatable chuck and has a trigger switch which controls the rotational speed of the electrode 13. The speed is variable between 5000 and 10 Ό00 rpm «,

The electrode 13 consists of the material to be fused with the matrix. The matrix or substrate for which the method is to be used and which is to be treated is designated 14. The matrix is also connected to the other side of the oscillator output through a terminal 15 and line 16

These connections make the electrode positive and the matrix negatively charged when the signal is applied »

In Fig. 2 sind.die corresponding components are numbered accordingly. But in this embodiment, the process used can be characterized as a liquid-by-solid process. In dieser.Anlage, the material to be fused form e / aüfuna is in -this container · -17. The container 17 is through a tube 18 with an electrode. 19 connected. Electrode 19 is a plate provided with an insulated handle 20 to which one side of the output of oscillator 11 is connected. This output is fed into a main channel 21 in electrode 19. Channel 21 is provided with a series of side channels 22 which are open to the bottom of the electrode 20. The flow from the container 17 is by gravity or by means of a pump and can be regulated by a valve as in 23 on the handle 20. to

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Further control, for more uniform distribution of the solution and for preventing the inclusion of foreign substances, the surface of electrode 19 is preferably coated with a permeable membrane such as cotton or rlylon.

It has been found that to achieve the merger

the application of 50 000 watts / cm or alternatively the application

a current of the order of 10 000 A / cm is required. ,

As a practical matter, 10,000 A / cm can not be applied consistently without damaging the matrix to be treated.

However, it has proved feasible to apply a pulse signal of 2.5 A to 28 A for a duration of 3 A to the electrode for a period of 2.5 seconds to 28.6

2 melt on an area of approximately 0.3 mm.

To complete a fusion on a surface with the equipment shown in Fig. 1, the electrode 13, matrix Η and the oscillator output are connected together as shown.

The worker performs the rotating electrode 13 ₅ communicating with the surface of the matrix in contact with a certain speed on the matrix surface, to deposit the electrode material on the matrix and to fuse it.

It has also been found that the continuous application of an alternating signal generates considerable heat in the substrate or matrix, and to eliminate this accumulation of heat and avoid welding, the signal generated in the system according to the invention is a half-wave signal enabling the dissipation of heat ,

As known to those skilled in the art, each material, both the matrix and the material to be applied, has resistivity characteristics. Thus, any change in either or both of these substances will be associated with a change in the resistivity of the circuit.

In Fig. 3, R = the resistance of the electrode

R ₂ = the resistance of the matrix and Ro = the resistance of the circuit of 10 and

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A change of R .. and R ₂ becomes changes of Fre- '. frequency of the generated signal and the amplitude of this signal.

As already mentioned, it is assumed by a signal with an amplitude of 3 A that ea has the preferred amplitude. If the amplitude is higher, decarburization or burning of the matrix occurs, and at lower amplitude, hydroxides are formed in the interface.

Pig. 4 is a schematic diagram of an oscillator circuit as applied to a system according to the invention. "

In this Stromkreia iat a power source 30 connected to the input and to the input a capacitor 31 is angeachloaaen. One side of the capacitor 31 is connected to the LC power circuit 32, which includes a control battery 33 and a condenser 34, which are connected in parallel.

The LC Stromkreia 32 is connected to one side of a crystal oscillator circuit comprising crystal 35, inductor 36 »UPN transistor 37 and the RC circuit with the variable resistor 38 and the capacitive resistor 39.

The oscillator array is connected to the output 50, and zviar on one side by the condenser 40 and at the

/ - \ other. Page through diode 41, to generate a half-wave * - "" signal at the Auagang 50.

In the actually used plant / the individual components had the following characteristics

31 = 1.2 / U-Parad

32 = 0.3 picofarad

33 = 0 - 25 millihenry

35 = 400 - 30 kHz

36 = 20 millihenries

37 = IPN

38 = 3.5 / U Farad

39 = 0 - 500 0hm

40 = 400 / U Farad

41 = diode

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To keep the amplitude of the signala at 3 A, R ^ resistance 38 is varied; Drosaelapule 33 is varied to change the frequency.

If C = the capacitance of the circuit of Pig «3 and R-, Rp and R ^ are the resistances characterized above, then one can assume that the optimum frequency is the melt signala

F can be determined from the following formula ο °.

F Formula I

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where L = ILeRo «Ro

and G = capacitance of the circuit «

L and C can be determined by any well-known method.

F depends on the material to be treated and the material to be applied, but will be in the range of 400 Hz to 35 MHz. It is believed that the frequency determines the speed of the process.

For merging, a certain area the same is measured,

Since approximately 0.3 mm are melted by each discharge, the Vorachub velocity is determined by the following formula:

_Feed rate = " _{pormel ιχ}

^ 4 ^. and

2 A = area to be coated in mm F = the number of discharges per second.

As explained above, the resistances R and Rp can be measured by any known method »

However, it has been discovered that the mechanism of resistance in the liquid phase may not be consistent. In this case, the resistance is measured using a standard method. Two electrodes at a distance of 1 cm and

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with an area of 1 cm are placed in a bath of the liquid phase and the resistance is measured after a delay of 20 seconds. After the variable parameters have been determined and the equipment, matrix and probe have been connected as shown in Figures 1 and 3, the probe 13 is passed over the surface of the matrix at the specified speed, touching the same »

The speed is also believed to affect the quality of fusion, with a surface finish in a non-uniform 200 to 300 / μm design being achieved at a speed of 5000 rpm, and surface finish at a speed of 10,000 rpm essentially has a 15 / um execution.

The plant of Pig. 2 vsird in the same way as the attachment of.Fig. 1, and the process is essentially the same, except that a liquid with a solid electrode is used

The procedure will become even clearer from the following specific examples. «

In each of these examples, the electrode was connected as shown in the description, so that after charging the electrode is positive and the matrix negatively charged.

The solid-by-solid process is exemplified by the examples. I, II, HA, III and IV illustrate *

Example I

Tool steel ^ Atlas A151 OT 'was connected as matrix 14 to the plant of Fig. 1, and as electrode 13- was used as titanium carbide designated as Kennametal K165.

The following are the characteristics and treatment conditions:

Matrix resistance 0.002 ohms

Probe resistance 0.026 ohms

Circuit resistance · 0.01 ohms

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Frequency (F ₁ ) 12 kHz at 4.62 yU Farad

Voltage 3 volts

Application speed 50 cm / minute

Treatment depth # 40 / um

Surface thickness increase £ 0.5 / um

The results from the treatment of the tool steel Atlas A151 01 with the titanium carbide are shown in the micrographs and the spectrometer scans of Fig. 5 to Fig. 17.

The polished and titanium carbide-treated steel was examined by means of SM / BPMA and showed the appearance of Fig. 5 °. From each of the numbered locations indicated in Fig. 1, X-ray images were taken and these are shown in the graphs of Figs shown and they correspond to the points 1 bia 8, respectively.

Figures 9, 10 and 11 represent spectra of the parent metal.

Figures 12 to 16 show the presence of a small titanium cap whose height did not change appreciably when crossing the zone.

As is apparent from Fig. 6, the approximate width of the zone in which titanium was detected is about 50 / μm, although this dimension changed with the length of the probe.

TJ nte coverage of the top surface layer using a microprobe analyzer gave the Ti-Kd X-ray image shown in Figure 7, which shows that the amount of titanium was fairly constant to a measured depth of about 40 / um was.

The sample was then covered with a thick coat of Mckel and polished again. As can be seen from Fig. 5, the custom built scanning micrograph showing a surface layer approximately ^1/2 micrometers. Fig. 17 is an X-ray spectrum of this layer.

A hardness test of the coated steel sample was then carried out and the results listed in Table I were determined.

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Table I

Knoop-hardened beats, load 100 grams enriched zone 650 (2) distance to the test piece edge KHN   536 516 (Inch) (D 655 728 0,0005) _Ti 790 770 0.001) 863 872 0.0015) 955 1006 0,002 536 1006 0.0025 243 453 0,003 - 0,004 148 0.005 0.01

As you will notice, the hardness characteristics of the steel have been significantly improved.

Example II .,

1018 steel was connected to the system of Fig. 1 as the matrix 14 and served as the electrode 13 of molybdenum, type Mo 1, the steel was 72 inches wide, Y χ 4 inch thick χ 1 ^1/2 inches long, the molybdenum 1 inch long at a diameter of 4 mm. The applied frequency was 43-31 kHz and the rate of electrode rotation was approximately 12,000 rpm.

The surface of the steel was bia to a surface finish with a grain of. 600 ground. The electrode tip was passed by hand over the surface of the steel sample in straight juxtaposed lines. The process was repeated in 90 to cover the entire surface, and small beads of molten and resolidified material could be detected under light microscopy at 40x magnification.

As can be seen from Fig. 18, the fusion of molybdenum with steel is clearly seen _o

The results of electron microprobe scanning of the interface show that molybdenum is at least

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15 / um is present, as shown in the table below and Fig. 19 shows.

Depth, /around Dimensions% Mo 1 6.9 2 7.6 3 7.0 4 7.5 10 6.6 15 6.0

93.1 92.4 93.0 92.5 93.4 94.0

Microhardness measurements were made on the sample cross section and gave the following results:

Knoop hardness number load depth from the surface 493 200 g 30 yum

198 200 g 40, um

The average KHN of the untreated steel was 188. The hardness of the same steel after heating to 900 ⁰ C and water quenching was 285 (KHN) at 200 g "

Example HA

The same matrix and electrode and the same Verfahrensweiae as in Example II were in a. Frequency of 30.63 kHz and the same speed applied.

Small beads of molten and resolidified material were detected under the light microscope.

As shown in Fig. 18A, the fusion of molybdenum with steel was quite clear.

The results of electron microprobe scanning of the interface revealed that molybdenum was present to a depth of at least 50 μm, as shown in the table below and in Figure 19A:

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Depth., ,around Massed Mo Massed Pe 10 8.8 91.2 20 11.2 88.8 30 3.6 96.4 40 3.6 96.4 50 2.5 97.5

Depth, /Around KM 15 375 25 506 40 445 150 227 500 188

Knoop microhardness measurements were made on the cross section of the sample. The following results have been obtained

Load 200 200 200 200 200

The hardness values in Examples II and HA above KHH 285 result from the presence of molybdenum.

Example III

Steel having the same specifications As in Examples II and HA, matrix 14 was connected to the plant of Fig. 1, and tungsten carbide (Kennametal type Ur. 68) served as the electrode 13. This electrode had a diameter of 5 mm and was 1 inch long.

The applied frequency was 26.20 kHz and the rate of electrode diffusion was approximately 12,000 rpm.

As a procedure, the same viie was used in Examples II and HA »

As is apparent from Fig. 20, tungsten was fused with the steel matrix. The results of electron microscopic analysis of the sample show that tungsten bia is present to a depth of at least 80 μm, as can be seen from Fig. 21 and the table below:

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Massed Fe

75.6.

72.5

98.3

98.2

98.9

98.3

Knoop microhardness measurements were made on the sample cross-section. Ea the following results were determined:

Depth, /Around Mass% W 1 24.4 5 27.5 10 1,7- 20. 1.8 50 1.1 80 1.7

Depth, / um KHH 28 908 45 718 T5 329 120 220

burden S 200 G 200 S 200 G 200

The hardness of the untreated sample is approximately 188 KHi and after heating to 900 ⁰ C and quenching at 285 KHN.

In addition to the above, it is clear that the surface hardness is improved by the treatment of the steel matrix, and that it is very useful for those cases where surface hardness plays an important role. "

For fusing a second conductive chemical element into the solid matrix of a first conductive chemical element using a solution of the second conductive chemical, as well as for each solution, the process was carried out at ambient temperature, 20 G, in the following manner.

The metal matrix 14 was connected to the circuit as described above. The frequency was determined according to the formula given above, and the solution contained in the container 17 was applied by passing the electrode over a surface of the first metal for different lengths of time, as determined by formula II. In order to ensure even distribution of the second metal solution on the surface of the first metal, the electrode was covered with tree gauze or lylon. It is clear that other substances can be used. This measure also served to reduce the contamination of the solution when using graphite

"limit" electrodes. With these, there is the possibility that "graphite particles will detach in the course of the movement".

The treated samples were then sawn to obtain a cut sample, washed in cold water, cleaned with ultrasonics, embedded in plastic, and ground and polished to obtain a flat surface and a smooth edge. For other samples of softer metals, where there was a risk that the edge would break off during grinding, two sections were bonded to the treated surfaces, as previously embedded and ground and polished.

After embedding, the sample was etched.,. for steel, the iron-containing substrate, Hital and for copper, the non-ferrous substrate, ammonium hydrogen peroxide was used »

In the course of some application work, it was found that sometimes adjustments of either the frequency or the speed of application were required. These had become necessary as a result of changes in solution composition or deviations in the matrix.

Semi-quantitative electron probe microanalysis of the fused interfaces was performed using Energy Dispersive X-Ray Spectroscopy (EDX) and a Scanning Microscope (SEM).

The surface of the embedding paste was made conductive by depositing an approximately 20 μm thick carbon layer on it in a vacuum evaporator. This measure was taken to prevent the build up of electrical charges on an otherwise non-conductive material and the resulting instability of the SEM image. Carbon which does not produce EDX detectable radiation was preferred over a more conventional metal coating to prevent interference of such a coating in elemental analysis. "

The operating conditions of the SEM were chosen so that interference and continuum radiation were kept to a minimum and at the same time the best possible spatial resolution was achieved. «

10 - 20 kV 2000 Hz 200 - 300 180 s 50 nm 100 - 300 pA 12 - 34 mm. 5000 - 10 000 perpendicular to the beam 225 ° 800 - 60 -

The general conditions used for elementary analysis by EDX are as follows:

acceleration potential

end opening

spot size

Beam current _n

working distance

magnification

Test specimen angle '

derivation angle

count rate

Time under tension

Energy calibration was tested using Al-Kd emission at 1.486 keV and Gu-K at 8.040 keV.

A standard semi-quantitative analysis was used to determine the elemental concentration using certified (UBS 478, 78 % Gu-27 % Zn and NBS 479a, Έί, 11 %, Gr 18 %, Fe) reference materials to confirm the results. Multiple cover analyzes were in excellent agreement with the confirmed values of NBS. An average accuracy of + 1 % was achieved. A size of analyzed volume was calculated from the following equation 1:

pfi _Cx) = 0.064 (E _O 1 ⁶⁸ - E ₀ J ⁶⁸ ).

in which mean

R / \ = the mass range (the X-ray generation volume) ρ = the density of the analyzed material E _Q = the acceleration potential

E = a critical excitation energy

The diameter of analyzed volume was calculated for typical analyzed elements and determined as follows: Ii 0.46

Cu 0.39

Fe - 0.55

W 0.30

23671

To determine the depth of diffusion, a static beam was passed over the interface at intervals greater than the above mass range. This ensured the accuracy of the analysis.

The "element concentration results were reported in masses for each point measured at the confluence interface

In the various examples that will be described, the second conductive chemical element is d, h. the element to be diffused into the matrix exists. In some solutions

Are there even small amounts of metal ions? One takes

& th £ $ c / sv irsH / ig fatlS

indicate that these metal ionVaTs complexing agents must be present to facilitate fusion. Small amounts of organic catalysts such as acacia, hydroquinone, bone glue, pepsin, dextrin, licorice or their equivalents may also be present.

Wetting agents such as sodium lauryl sulfate or its equivalent are normally used.

If necessary, pH modifiers such as ammonium hydroxide or sulfuric acid are usually added to achieve the required pH.

Some other solutions require complexing agents for the second chemical conductive element which preclude precipitation of the second element. Such agents are, for example, citric acid or sodium pyrophosphate or ethyldiaminetetraacetic acid or their equivalents *

In some solutions, a suitable buffer is also provided, if necessary.

The water is always demineralized.

And for certain applications, where the appearance of the product must be appealing, small amounts of brightening agents such as. Formaldehyde, carbon disulfide ,. Benzolauronic acid or its equivalents can be used «

In these examples, unless otherwise stated, ASA 1018 steel matrix and ASTM B-i333 copper alloy 110 are used.

0.0018 ohms Ki Ioohm 0,4 picofarad 2 150 0.01 ohms cm / minute 650 Hz at , 5 / um 2αη 5 / um 60 · »O  \> '

Example IV

Steel Atlas Al 51 1020 was connected as matrix 14 to the plant of Fig. 2, and a 10% solution of ammonium molybdate in water was placed in vessel 17,

The following characteristics and treatment conditions were used:

Matrix resistance ⁺ Probe resistance Circuit resistance Fre quency Contact surface Speed Handling Deep surface elevation

+ 2

Determined by measuring 1 cm plates that were 1 cm apart, after a delay of 20 seconds,

The sample of Example IV was subjected to a thermal corrosion test. 25% sulfuric acid was allowed to act on the surface for 20 minutes at 325 G without any surface penetration.

Example V

It was an aqueous solution having the following composition

made: '~

lame grams / liter

Sodium molybdate 37> 8

Iron (II) ammonium sulfate 7

Iron (III) ammonium sulphate 8.6

Citric acid 66.0

Water (distilled) 997 ml

Sodium lauryl sulfate 0.5

Ammonium hydroxide to the required pH

Acacia gum (gum arabic) 0.1-0.2

Formaldehyde. 7.5 ml

The solution showed the following characteristic value

- ^Hb - L όΌ / IU L ·

pH = 7.5

resistivity = 19 ohm-cm

Mo ⁺ concentration = 1.8 mass

Fe ⁺² = 0.10 mass

Pe ⁺³ = 0.10 mass

The concentration of Mo ⁺ can be varied from 1.5 to 2.5 masses; the pH can be from 7.2. "to 8.2 and the resistivity can be between 17 and 25 ohm-cm"

Reaction derivatives

Matrix = copper

Electrode = graphite

Electrode cover = cotton fabric

Frequency = 9.09 kHz

Application speed = 736.2 mm / minute

Application time = 2 minutes

It is believed that in the "explained VT solutions, the presence of" in Examples V and Eiaen (II) - * · ion serves the Wertigkeitszustand'von Mo ⁺ to - and E is en ^(HI): a geringeren- to reduce the activity factor * ·

Although the iron appears to be transferred simultaneously, as shown in Pig. 23, the iron evidently exerts no material influence on the characteristics of the matrix or molybdenum.

An examination of the sample with a light microscope shows a continuous molybdenum coating which is free of pitting and has a dark silver coloration.

As in the table below and Jig. 23, it is apparent from an SEM / EPMA scan of the interface between the matrix and the deposited metal that molybdenum has been fused to a depth of at least 4 μm at a surface deposition of approximately T / μm.

Table depth, / element ' concentration (mass)

0,5 - · Mo - · 65,4

Pe 19,9

Gu 1.4.5

1.0 Mo. 58.4

Pe 10.9

About 30.5

2.0 Mo 6.6

Pe 0.8

Gu 92.5

3.0 Mo 2.9

Pe 0.4 Ca. '96.6

4.0 Mo 0.9

Pe. 0.0

About 98.9

example

Ea, an aqueous solution having the same composition as in Example 1 was prepared and made into the following conditions. "

Reaction conditions

Matrix ": = steel (ASA 1018)

Electrode = graphite; -

Electrode coating. = Cotton fabric

Preqaenz = 4.11 kHz

Application speed = 739.8 now / minute

Duration of application = 3 minates

Examination under the light microscope revealed a continuous dark silver colored surface.

The micrograph of Pig. Figure 24 shows the deposition of a substantially uniform layer of molybdenum in a thickness of 1 / am and with uniformity.

Like from Pig. 25, an SEM / EFMA scan of the interface between the substrate and the deposited metal shows that molybdenum was present to a depth of at least 10 microns "with a molybdenum gradient as shown in the table below."

Table Depth, / around Element Concentration (Massel)

0.5 - "Mo 81.0

Pe 19.0

2 Mo Fe 3 Mo Fe 10 Mo Fe Example YII

2.2 97.8

0.8 99.2

0.6 99.4

Ea an aqueous solution with the following composition was prepared

Urine . Grams / liter

Uatriam tungstate 31,40 ~~ '

Ferric ammonium sulphate 8,63

Eiaen (II) -aulfat 4.98

Citric acid 66,00

Water (distilled) 1000 ml

immonium hydride "" to the required pH

/ Sodium lauryl sulfate 0.1 '

Formaldehyde 5 ml

The solution had the following characteristics

pH value "" 7.99

resistivity = 22 © hm-cm

W * ⁶ x = 1.75 mass

Fe ⁺² _ = 0.1 mass

= ©, .1 Massel

The W ^TVJ concentration can vary between 1.6 and 2.5 ^mass ; the; pH may be from 7.5 "to 8.5" and the resistivity may be between 18 ohm-cm and 24 ohm-cm.

Reaktionäredingungen

Matrix '' - · - · = copper

Electrode = graphite

Electrode cover = cotton gauze

Frequency = 3.83 kHz

Application speed = 689.4 mm / minute

Duration of application. = 3 minutes

? / ie can be seen from the micro-images of FIGS. 26 and 27,

lab / ! U

Fe Ca 38.5 24.2 2.1 93.1 O _t 3 99.2 0.2 99.1 0.2 99.5

The sample showed a uniform tungsten layer with a thickness of approximately 1 micron. Erne SEM / SPMA scanning showed a tungsten-to-copper-to-fusion to a depth of at least 5.0 micrometers, as shown in the table below and FIG. 28 can be seen.

Table . ".

Depth, around concentration (Massel)

1.0 37.3

2.0 4.8

3.0 x 0.5

4.0 0.7

5.0 '0.3

Example VIII

It became an aqueous; solution prepared with the following composition:

CTame . Grams / liter

Matriumvolthrate 34.00 '"

Iron (II) sulphate ¹ .. 4,98

Egg (II) ammonium sulfate at 7.02

Iron (III) ammonium sulphate 8.62

Citric acid. 66,00

Water (distilled) 980

Ammonium hydroxide "to the required pH sodium lauryl sulfate 0.10"

Annotation; It can be used either 1 or 2.

The solution had the following characteristics: pH * = 8

resistivity = 20.9 ohm-cm

W ⁺⁶ = 1.9 mass

= 0.1 mass = 0.1 mass

The concentration of tungsten can vary between 1.6 and 2.5 masses; the pH can be from 7.5 to 8.5 and the '

apecific resistance can range from 18.8 ohm-cm to 22.8 ohm-cm.

HeaktJonabedindungen

Matrix = steel (ASA 1018)

Electrode - = graphite

Electrode coating = Baamwollgaze

Frequency = 4.78

Application speed = 860.4 mm / minute

Application time = 3 minutes

An examination of the sample with the help of SEM / ΕΡΜΑ, Pig. 29, showed a T / olframachicht of approximately 0 ^ 5 / um, and as with Pig. 30 and the subsequent table, tungsten bia could be detected to a depth of at least 3 / um

^earth table Concentration (mass) The solution had the following characteristics "= 1.60 Depth, um element PH value = 51.8 ohm-cm '/'. '0.5 "' W 6 specific resistance = 1, 75 mass 1 W 1 Concentration In ⁺ .:. '' / · ', .':. ·,.,. , 'γ-, - * ''. * '* "" ^: .;', = 0.077 mass 2 W 1 * 1      . ·. , : .- ·; ·. , .: .. · ... . '' '4-3 Concentration Al 3 W. ' Beiapiel IX following composition It was "an aqueous Löaung with hergeatellt: Grams / liter Surname 40.0 "- Indium's ulf at 9.6 Aluminum sulphate at 3.5 Sodium sulphate · 0.05-0.1 gelatin 0.1-0.2 Natriumlaurylaulfat 1000 ml Water (distilled)

The indium concentration can vary between 0.2 and 2.2 masses; the pH may be from 1.60 to 1.68 and the resistivity may be between 48.8 ohm-cm and 54.8 ohm-cm.

Reaktionabedingungen

Matrix ~ '= copper

Electrode = graphite

Electrode cover = cotton gauze

frequency = 4.75

Application speed = 855 mm / min

Ordering time = 3 minutes

An examination of the sample under the light microscope and the scanning microscope showed a continuous surface that was free from structural defects, such as Pig. 31 shows *

As shown in the table below and Figure 32, an SEM / ΕΡΜΑ scan of the copper matrix-indium layer interface revealed a plot of approximately 1 / μm and a fusion of indium to a depth of at least 4 / μm ,

' Table

Depth, / um 1 element Concentration of indium ι 2 (Pig) 3 In 90.3 4 In , 5, .5 Example X In 4.3 In 3.6

Is, the solution of Example IX was used and applied to a steel matrix: reaction conditions

Matrix = steel (ASA 1010)

Electrode ~ = platinum

Electrode overlay = nylon fabric

Frequency = 6.29 kHz

Application speed = 1132.2 mm / minute

Duration of application = 3 minutes'

Like the pig. 33 and 34, a smooth continuous layer of indium was deposited on the surface of the matrix to a thickness of approximately 1 μm. An SEM / SPMA scan, Figure 34 'of the interface and the table below, show a fusion to a depth of at least 3 / um.

table

Depth, /around In (Pig) Pe (Massel) 0.5 91 4 8.6 1.0 5, 2 94.8 2.0 1, O 99.0 3.0 O, 9 99.1

Pig, 35 shows a solid nickel layer of uniform density and thickness of approximately 1.5 / μm. As the following table and Pig. 36 illustrate, an SEM / ΕΡΜΑ scan of the interface between the matrix and the nickel layer showed that nickel fused to a depth of at least 4 / um

pig

92.6 '

; 4.5

3.3

1.0

Ea was prepared an aqueous solution having the following composition:

Name grams / liter

Nickel (II) sulfate 248.9 '"

Nickel (II) chloride 37.3

Boric acid ", 24.9

Formaldehyde 3 ml / liter

Benzolauronic acid 10 ml / liter

Sodium lauryl sulfate 0.1

Water (distilled) 900

has been. element Depth, / um Ni 1 Ni 2 Ni 3 Ni 4 Example. JI

4- WW / 3 W im

The solution had the following characteristics:

pH = 3.10

Specific resistance = 22.5 ohm-cm

Concentration of Hi = 6 pigs

The nickel concentration can vary between 2 and 10 % ; the pH may be from 3.10 to 3.50 and the resistivity may be between 17 ohm-cm and 26 ohm-cm.

Reaktionabedingungen

Matrix = copper

Electrode = graphite

Electrode cover = cotton gauze

Frequency = 7.50 kHz

Application speed = 1350 mm / minute

Application time "= 3 minutes

Beiapiel XCI

The same solution was prepared as for Example XE and applied to a steel matrix:

Reaktionabedingungan

Matrix '= steel (ASA 1018)

Electrode = graphite

Electrode cover = cotton gauze

Frequency '= 7.50 kHz

At transmission rate = 1350 mm / min

Application duration = 3 minutes

As shown in Fig. 37, the efickel layer is continuous and exhibits a substantially uniform thickness of about 1.5 / μm.

As shown in Fig. 38 and the table below, nickel bia was fused to a depth of at least 3 / μm,

Depth, / around element concentration (Massel)

1 Ni 95.9

2 Ni 28.0

3. , Ni 0.7

2 36 7 10 2

Example XEII

Sa became an aqueous solution having the following composition

manufactured:

Harness grams / liter

Gold chloroacetic acid 2.5

Potassium ferrocyanide 15jO

Karlimcarbonate 15.0

Water (distilled) 1000 ml

This solution had the following characteristic value pH = 10.99

resistivity = 40 ohm-cm

Concentration of Au ⁺ ions = 0.14 mass

The pH can be varied between 3 »70 and 11; the concentration of Au ⁺ ions may be from 0.1 to 0.5 mass and the resistivity may be between 40 ohm-cm and 72 ohm-cm.

Reaktionabedindungen

Matrix "., = Copper

Electrode = platinum

Electrode coating. = Cotton gauze

Frequency i 4.33 kHz

Application speed = 779.4 mm / minute

Application time = 2 minutes

Examination with the aid of the light and scanning microscope revealed a surface layer of gold approximately 1.5 μm thick, which was continuous and uniformly dense, as shown in Pig.

An SMM / EPMA scan of the interface showed a fusion of gold to a depth of at least 3 / um as shown in the table below and Pig. 40. is.

Depth, in element , concentration (mass)

0.5 Au T, 0 Au 2.0 Au 3.0 Au

61.3 9.6 0.9 0.5

/ IU

Example XIV

An aqueous solution having the same composition as that of Example XIII was prepared.

reaction conditions

Matrix = steel

Electrode. = Graphite

Electrode coating. = Cotton gauze

Frequency = 3.95 kHz

Application speed = 711.0 mm / minute

Application duration '= 2.0 minutes

Examination with the light and scanning microscope revealed a gold layer on the surface with a thickness of approximately 1.0 μm. The layer was uniformly thick and dense, as shown in FIG. 41.

An SEM / EPMA scan of the interface showed a fusion of "gold" to a depth of at least 4.0 / μm as shown in the table below and FIG. 42.

Depth, by element concentration (%)

0,5 Au 84,9

1.5 Au 10.6

2.0 Au 2.1

3.0 Au 0.8

4.0 Au 0.6

Example XV

An aqueous solution with the following composition was prepared:

Name - grams / liter

Chromium trioxide. 150 -

Chromium sulfate 0.06

Sulfuric acid 2.15

Sodium hexafluorosilicate 0.2

Carbon disulfide id 2 - 3 ml

Sodium lauryl sulphite 0.05

Water (distilled) 'to 1000 ml

The solution had the following characteristics: pH '' = 0.6

resistivity = 12 ohm-cm

Concentration of Gr ⁺ = 7.8 mass

The pH can be varied between 0.6 and 1.0; the concentration of Gr ions may be between 3 and 20% by mass and the resistivity may be between 11 ohm-cm and 14 ohm-cm.

Reaction conditions -

Matrix · = copper

Electrode = graphite

Electrode cover = cotton gauze

Prequency = 6.25 kHz

Application speed = 1125 mm / minute

Application time = 5 »0 minutes

Light and scanning microscope studies have shown a Ghrom layer on the surface of approximately 1 / μm thickness. The surface of the layer was irregular, but the layer appeared to be free from imperfections and was continuous, like Pig. 43 shows.

An SEH / EPMA scan of the interface showed that chromium was fused to a depth of at least 3.0 μm, as shown in the table below and Pig.

Depth, / um element Concentration (mass) 0,5,: Gr 94.0 1.0 Gr 32.0 2.0 Gr 1.8 3.0 Gr 1.0 Example XVI

An aqueous solution of the same composition as used in Example XV was prepared:

Reaktionabedindungen

Matrix ^; = Steel (ASA 1018)

Electrode = graphite '· -

U -

Electrode coating = Bauinwollgaze

Frequency = 6.48 kHz

On tragunga gea chvs ind igke it = 11 66, 4 mm / minute

Application duration = 5.0 minutes

Examination with the light and razor microscope revealed a chrome layer on the "surface with a thickness of approximately 3.0 μm, corresponding to that shown in Pig" 45.

An SEM / ΕΡΜΑ scan of the interface showed a fusion of chromium bia to a depth of at least 5.0 / μm, as shown in the table below and FIG. 46.

Depth, / um element Maaae% 1.0 Cr 100 2.0 Cr 97.2 3.0 Cr '20,8 4.0 Cr 2.8 5.0 Cr 2.1

Example XVII

An aqueous solution with the following composition was prepared:

Ή ame '· grams / liter

Chromium (Ui) chloride. 213: ^""

Sodium chloride 36

Ammonium chloride 2.6

Boric acid 20

Dimethylformamide 400 ml

Sodium acetate 3.0

Sodium lauryl sulfate 0.5

? / Ater. (distilled) to 1000 ml

This solution showed the following characteristics:

pH value = 3.0

resistivity = 17.4 ohm-cm

Concentration of Cr ⁺ = 2.5 bia 3.5

The pH can be varied between 2.5 and 3.5; the

Concentration of Cr ⁺ ions can be between 1.8 and 5.0 mass

ZJD / i U I

and the specific resistance may be 16 ohm-cm to 20 ohm-cm.

Reaktionäredindungen

Matrix = copper

Electrode = graphite

Electrode cover = cotton gauze

Frequency = 6.85 kHz

Application speed = 1251 mm / minute

Application time = 3.0 minutes

Examination with the light and scanning microscope revealed a chrome layer on the "surface of approximately 0.5 / μm thickness." The layer, mar feat and continuous as Figs. 47 and 47A 'show.

An SEM / ΕΡΜΑ scan of the interface revealed a fusion of chromium bia to a depth of at least 3.0 , as shown in the table below and FIG. 48.

Depth, / around element concentration (Massel)

1 - Cr, 21.2

2 Cr 4.0

3 'Cr 0.9

Example XVIII

Ea was an aqueous Löaung with the same composition as prepared for Example XVII was used:

Ectictive Indications

Matrix. , = Steel (ASA Ί0Τ8)

Electrode graphite

Elektrodehüberzug = cotton gauze

Frequency = 6.85 kHz

Application speed = 1251 mm / minute

Application duration = 3.0 minutes

The investigation with the light and Raatermikroakop resulted in a Chromachicht on the surface., Mit.-one. Thickness of approximately 1.0 / um. The surface of the layer appeared to be somewhat irregular, but the layer was firm and free of defects.

- 39 - ι JD / IU I

learn, Figs. 49 and 49A show »

Bine SEM / ΕΡΜΑ-Aldtastung of the interface showed a fusion of chromium bia to a depth of at least 3.0 / um, as shown in the table below and Fig. 50.

Depth, / at element concentration (Massel)

0.5 gr 97.2

1.0 Cr 97.6

1,5 Cr. 22.2

2.0 Cr -1.5

3.0. Cr 0.8

example UX

An aqueous solution with the following composition was prepared:

Uame Gram m / Lite r

Cadmium chloride Sodium phosphate Phosphate (distilled)

The solution had the following characteristics: ρH value

specific resistance

- +2 ^ concentration of Cd

The pH can be varied between 10 and 10.2; the concentration of Cd ions may be between 0.2 and 0.5 mass, and the resistivity may be 28 ohm-cm to Qhm-cm.

reaction conditions

Matrix '= copper

Electrode = graphite

Electrode cover = cotton gauze

Frequency = (1) 7.29 kHz;

- (2) 7.91 kHz 'application speed = (1) 1 312.2 mm / minute;

"(2) 1423.8 mm / minute"

6 74 10 ml 54 33 1000 P, 0hm-cm _ 32 pigs  77

- 40 - I ά Ö / IU L

Plot duration = (1) 1.0 min;

(2) 3.0 min.

In this example, the solution used was initially that described above, which was applied according to the conditions indicated as (1). A second solution, cited in example ΧΣ, was then applied under the 8.1s (2) labeled conditions.

Examination with the light and scanning microscope revealed a cadmium layer on the surface with a thickness of approximately 4 μm. This layer was as.! 51, not homogeneous, but an SM / EPMA scan of the interface showed a fusing of cadmium to a depth of at least 9 / um as shown in the table below and FIG. 52.

Depth, / um element Concentration (mass) 2 CD 77.4 3 CD 65.2 4 CD 6.7 VJL CD 1.2 6 CD 0.48 7 CD 2.1 8th CD 2.9 9 CD 0.89 Example SX

It i iurde, _{a: aqueous:} solution prepared with the following composition ·;

urine Grams / liter cadmium sulfate 26.65 " sodium chloride .8,7 boric acid 15.0 aluminum sulphate 17.5 Acacia gum (gum arabic) 0.25 Sodium tetraborate 5.0 Benzenesulfonic acid ,. 2.5 Hatriumlaurylsulfat 0.5 Water (distilled) 1000 ml

O / 1 U I

This solution had the following characteristics: pH value = 3.40

resistivity = 54.0hm-cm

Concentration of Cd = 1.1 %

The pH can be varied between 3 »2 and 3 _} 5; the concentration of Cd ions can be from 1 "to 4% by weight and the resistivity can be between 45 ohm-cm and 55 ohm-cm.

reaction conditions

matrix = steel

Electrode = platinum

Electrode cover = Hylontuch

Fre quency '. = 13.7 kHz

Application speed '= 2466 mm / minute

Application time = 2 minutes

Examination with the light and scanning microscope revealed a cadmium layer on the surface with a thickness of approximately 1 / um. The. The surface of the layer was irregular, but it was solid and continuous, as shown in FIG. 53.

An SΕΜ / ΞΡΜΑ scan of the interface showed a fusing of cadmium to a depth of at least 4 / um, as shown in the table below and Figure 54.

Depth, / um element Concentration (mass) 0.5 CD 73.3 1.0 CD 8.8 2.0 CD '1.4 3.0 CD 1.2 4.0 CD 1.1 Example XXI

An aqueous solution with the following composition was prepared:

Name grams / liter

Tin (II) chloride 77.3 *

Sodium hydroxide 66.0

3 % y

Sodium acetate 14,7

V / asser (distilled) 1000 ml

This solution had the following characteristics; pH "= 12.4

Specific resistance = 8.6 ohm-cm

Concentration of Sn ions = 4 pigs

The pH can be varied between 11.2 and 12.7; the

+ 2 -

Concentration of the Sn ions may be between 2 and 5 mass%, and the resistivity may be 6.2 ohm-cm to 10.3 ohm-cm.

Reception procedures

Matrix '= copper

Electrode. = Graphite

Electrode cover = cotton gauze

Frequency = 9.85 kHz

Application speed = 1773 mm / minute

Application time = 2 minutes

Examination with the light and scanning microscope revealed a tin layer on the surface with a thickness of approximately 1.2 μm "The layer was uniformly thick" and "homogeneous." This is evident from FIG.

An SEM / EPMA scan of the interface resulted in a fusion of tin to a depth of at least 4 / um, as can be seen from the table below, and Figure 56.

Concentration ¹ (mass ?!) 91.4

4,4:

0.9 0.5

Example ΣΣΙΙ

It was an aqueous solution having the following composition

manufactured:.

Depth, / um element 1 sn Second sn 3 sn 4 sn

ΙόΌ

Surname Grams / liter Characteristics: = 9.05 Tin (II) chloride 9.4 - = 34mm-cm sodium diphosphate 44.7 dextrin 6.25 Water (distilled) 1000 ml Sodium lauryl sulfate at 0.5 This solution had the following PH value specific resistance

Concentration of Sn = 0.50 mass

The pH can be varied between 9 and 9.7; the concentration of Sn ions can be between 0.4 and 1 mass and the resistivity can be between 30 ohm-cm and 36 ohm-cm.

reaction conditions

Matrix = copper

Electrode = graphite

Blektrodenüberzug = cotton gauze

Frequency = 9.85 kHz Application rate - = 1773 min / minute

Application time = 2 minutes

Examination with the light and scanning microscope revealed a tin layer on the surface with a thickness of approximately 4 / um. This plot appears to consist of a "lower uniform and substantially homogeneous layer having a thickness of approximately 1 μm and an outer slightly porous layer having a thickness of approximately 3 μm, as can be seen in Pig, 57.

An SEM / ΕΡΜΑ scan of the interface resulted in a fusion of tin to a depth of at least 5 / um as shown in the table below and FIG. 58.

Depth, / um element Concentration (mass ?!) 1 sn 97 IV) sn 97.3 3 sn 94 ', 3 5 sn 1.0

- 44 - / < y

Example XXIII

An aqueous solution of the same composition as prepared for Example XZII was used:

Reaction conditions .

Matrix = steel (ASA 1010)

Electrode = graphite

Electrode cover = cotton gauze

Frequency = 10.61 kHz

Application speed = 1909.8 mm / minute

Application time = 3 minutes

Examination with the light and scanning microscope revealed a tin layer on the surface with a thickness of over 2 / μm. This layer was porous but continuous, as shown in FIG. 59.

An SEM / EPMA scan of the interface resulted in a fusion of tin to a depth of at least 2 / um, as can be seen from the table below and FIG. 60.

Depth, / um element Dimensions% 0.5 sn 96.2 1.0 sn 81.4 2.0 sn 2.5 Example XXIY

It was an aqueous solution having the following composition

manufactured:

Uame ·

Cobalt (II) sulfate sodium fluoride boric acid

dextrose

Matrium lauryl sulfate water (distilled)

This solution had the following characteristic values pH value '

resistivity concentration of Go

Grams / liter ml 252 03 14 , 5 ohm-cm 45 3 massed 5 0.2 1000 = 6, = 28 = 5,

L Ö D / i Ua

The pH can vary between 4.5 and 6.5; the concentration of Go ions can be 2 to 6 masses and the specific resistance can be between 25 ohm-cm and 30 ohm-cm.

reaction conditions

Matrix "= copper

Electrode = platinum

Electrode coating = nylon waste

Frequency ._._ .. = 5 »1 kHz

Application speed = 918 mm / minute.

Application duration = 3.0 minutes

Scanning with the light and scanning microscope revealed a cobalt layer on the surface with a thickness of approximately 6.5 / μm. This layer was uniform and continuous, as shown in FIG. 61.

An SEM / EPMA scan of the interface showed a fusion of cobalt to a depth of at least 20 μm, as shown in the table below and FIG. 62.

Depth, / around element concentration (Massel)

10 Go 2.65

15 Go 1.6

20 Go 0.87

25. Go 0.44

From the visual examination and the preliminary experiments, it was found that the deposition of cobalt was extremely dense at a level of over 10 Ω / □.

Example 2X7

Ea became an aqueous solution with the following composition

manufactured:

Name ' grams / liter

Silver cyanide. 26 "

Kai i urne y an id 46

Potassium carbonate 37

Sodium Laurylaulfate 1

Carbon disulfide 1, -2

Water (distilled) 1000 ml

This solution had the following characteristics; pH "= 11.55

resistivity = 10.5 ohm-cm

Concentration of Ag ⁺ = 2.09 mass

The pH can be varied between 11.2 and 11.7; the

+ 1

The concentration of Ag ions may be from 1 to 3 masses and the resistivity may be between 8 ohm-cm and 13 ohm-cm.

reaction conditions

Matrix = copper

Electrode = platinum

Electrode coating = nylon

! Frequency = 7.7 kHz

Application speed. = 1386 inm / minute

Application time = 1.0 minute

Examination with the light and scanning microscope revealed a silver layer on the surface with a thickness of approximately 5 / um. The figure can be seen in Figs. 63 and 63A.

An SELi / EPMA scan of the interface resulted in a fusion of silver to a depth of at least 3 / urn, as shown in the table below and Pig. 64 can be seen.

Depth, / around element concentration (Massel)

1 Ag 98.7

2 Ag 91.4

3 Ag 46,3

4 Ag 2,4

5 Ag .1.0

Example ΣΣΥΙ

It became, an 'aqueous. Solution made with .following composition!

Name ' Gramm / Ljter

Silver nitrate 29

Potash iodide 398

Citric acid 6

Dextrose 5

Carbon disulfide 1.5

Ammonium hydroxide bia to pH

V / aaser (distilled) 1000 ml

This solution had the following pH value. '= 5.6

A specific resistor = 6.6 ohm-cm

Concentration of Ag = 1.84%

The pH can be varied between 1.5 and 2; the concentration of Ag ⁺ ions can be from 0.5 to 2.5 mass and the resistivity can be between 6 ohm-cm and 12 ohm-cm. lie.

Reactiona conditions

Matrix. = Copper

Electrode = graphite

Electrode cover = cotton gauze

Frequency = 9.5 kHz

Application speed = 1710 mm / minute

Application duration = 2.0 minutes

Scanning with the light and scanning microscope showed a silver layer on the surface with a thickness of approximately 2 / um. Daa texture is shown in FIG.

An SEM / EPMA scan of the interface resulted in a fusion of silver to a depth "of at least 2.00 nm , as shown in the table below and Figure 66.

Depth, / around element concentration (Massel)

1 Ag .97,7

2 Ag 97.5

3. 'Ag 28.0

4 Ag 3.8

5 Ag 2.8

6 Ag 1.0

As can be seen from the above examples, the invention provides a novel process, an apparatus for carrying out the process, solutions for use

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the process and new products that are suitable for the most varied applications and conditions of use provided.

Although the description has been limited to examples in which application has been made on the entire surface, it is to be understood that the application may of course be limited to specific areas of surfaces depending on a specific desired result.

For example, tin, gold and silver can be used due to the excellent, ending cases for them typical conductivity characteristics for electrical Aim, and circuits can be fused to other substrates,

The anti-corrosive properties of tin, gold, silver, nickel, ghrome, cadmium, molybdenum and tungsten are also valuable. And the application of these metals to iron and light iron substrates will improve their anti-corrosion behavior,

Chromium, nickel, silver, gold or tin also offer the '• possibility' of giving the matrix a pleasant appearance. Chromium, molybdenum, tungsten, titanium and cobalt give the matrix surface hardness «

Indium adds strength to the matrix and also serves as an anti-chemical agent. A molybdenum-treated ferrous or non-ferrous matrix has improved friction wear and high temperature resistance characteristics and is also suitable as a dielectric coating.

A cadmium fused matrix not only has improved corrosion resistance characteristics but can also serve as an antifouling agent for ship hull treatment.

Overall, silver-fused matrices are valuable as a reflective medium.

It will be apparent that the process and plant can be used in a very versatile manner without great capital and equipment expense, and enable the use of materials in applications that have previously been of lesser value

Expenditure than previously did not come into question, and in addition to the application cases and applications described, "many others will be aware of this.

It will also be apparent that the various parameters of the method may be varied according to the variables involved and the results sought, without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (20)

^so 2 3b / i U L Erf indungaanapruch; A method for melting at least one second conductive chemical element having a matrix of a first conductive chemical element at ambient temperature, characterized in that the second conductive element is brought into contact with an adjacent surface of the first conductive chemical element and a chopped electrical Signal of a certain frequency to daa first and second chemical element is applied, whereby the second chemical element is fused with the first chemical element. 2. The method according to item 1, characterized in that the Signal a pulse signal in the range of 2.5 microseconds to 2 is 28.6 lanoaeconds with an amplitude of 3 A per 0.3 mm over a given period of time. 3. The method according to item 1, characterized in that the second conductive element is passed over the matrix at such a speed that a substantially continuous merging surface of the second conductive chemical element is formed with the first chemical element. 4. The method according to item .3, characterized in that the movement speed of the second conductive chemical element is substantially proportional to half the frequency of the electrical signal. 5. The method according to item 2, characterized in that the frequency is in the range of 400 Hz to 35 MHz. A method according to item 1, characterized in that the first conductive chemical element is selected from the group consisting of ferrous and non-ferrous metals or an alloy thereof. A method according to item 1, characterized in that said second conductive chemical element is selected from the group consisting of iron or non-ferrous metals or an alloy thereof. 8. The method according to item 1, characterized in that the first conductive chemical element of the ferrous metals or an alloy thereof comprehensive group and the second conductive Element is selected from the non-ferrous metals or an alloy of the same encompassing group. The method according to item 1, characterized in that said first conductive member is selected from the group consisting of nonferrous metals or an alloy comprising the same, and said second conductive member is selected from the group consisting of ferrous metals or an alloy thereof. 10. The method according to item 1, characterized in that the second conductive element is in the form of a solid electrode containing the second conductive element, 11. Plant for fusing a first conductive chemical element with a second conductive chemical element, characterized in that it comprises a resonant circuit for the production of a chopped. Semi-wave signal within a certain frequency range, wherein the resonant circuit has an output and possibilities for the application of the resonant circuit output to a matrix of a first conductive chemical element to which a second conductive chemical element is fused ', and the second chemical element, whereby the second conductive chemical element is fused with the first conductive chemical element, 12. Appendix according to item 11, characterized in that the particular frequency is set. 13 · Installation according to item 11, characterized in that the specific frequency is variable and the system has possibilities to vary the signal. A product characterized in that it has a matrix of a first conductive chemical element having an outer surface fused to a second conductive chemical element at least on the outer surface and recovered by the method of item 1. Product according to item 14, characterized in that the first conductive chemical element is composed of the iron or non-ferrous metals or an alloy of the same group and the second conductive chemical element of the iron or non-ferrous metals L OO / 1 U L · Non-ferrous metals or an alloy of the same comprehensive group selected iat and differs from the first conductive chemical element. 16. Product according to item 15, characterized in that the first. conductive chemical element is ferric or an iron alloy. 17. Product according to item 15 , characterized in that the first conductive chemical element is non-ferrous or a non-ferrous alloy. 18. Product according to item 16, characterized in that daa second conductive element is non-ferrous or a non-ferrous alloy. 19. Product according to item 16, characterized in that the second conductive element is ferrous or an iron alloy. 20. A product according to item 16, characterized in that the first conductive chemical element is steel and the second conductive chemical element is selected from the elements of groups 4B, 6b of the periodic table. » 21 = installation for fusing an electrically conductive component with another electrically conductive component, characterized in that the system comprises an electrical power source, the power source comprising a resonant circuit and an output for providing a half-wave electrical signal at the output and the output a Klernmenpaar a first connection device connected at one end to an output terminal and having its opposite end connected to the other component at one location, and a second connection device connected at one end to the other output terminal and the opposite one End may be connected to the other component at another location, wherein the first connection device having the one component at the opposite end of the first connection device to bring the one component with the other component in contact when the ers te connecting device a.n it is connected and the electrical power supply is in operation and directs an alternating current through the components to fuse the one component to the other component. 22a system according to item 21, characterized in that the half-wave signal has a lying in the range of about 400 Hz to about 35 MHz frequency. Installation according to item 21, characterized in that the alternating current has a maximum value of about 3 A, and the first Connecting device that brings one component into contact with about OJ nan of the other component » 24. Plant according to item 21, characterized in that the other electrically conductive component is in solid form. 25. An installation according to item 22, characterized in that the first connecting device has possibilities for rotating the first component when it is in contact with the other component. 26. Appendix according to item 25, characterized in that the rotary device is actuated, it can be that the first component with a lying in the range of about 5000 to 10,000 rev / min 'lying speed. 27 · Plant according to item 21, characterized in that the other electrically conductive component is present in liquid form. An installation according to item 26, characterized in that the first connection device comprises a container for the liquid other component and means for regulating the flow of the liquid component into contact with the other component. Here are L-Seiien Zeichmingen