KR20050112520A - Method and composition for creation of conversion surface - Google Patents

Abstract

The present invention generally relates to the field of producing phosphate-metal chemisorption layers for iron and aluminum parts as well as other metal substrates capable of forming conversion surfaces. The phosphorus-containing solution is in contact with the metal component to form the transition surface.

Description

METHOD AND COMPOSITION FOR CREATION OF CONVERSION SURFACE}

Related Applications

This patent application claims priority to US Provisional Patent Application No. 60 / 443,995, filed Jan. 31, 2003 and US Provisional Patent Application No. 60 / 480,672, issued June 23, 2003. These priorities are all attached as references.

Technical field of invention

The present invention generally relates in particular to the field of the production of phosphate-metal chemisorbed layers for iron and aluminum parts as well as other metal substrates capable of forming conversion surfaces.

Background of the Invention

The production of iron-phosphate conversion surfaces is well known to produce surfaces that exhibit high dry lubricity, among other advantages. Creating an iron-phosphate conversion surface on an iron portion or part of an apparatus is typically accomplished through a phosphatizing bath process. Such baths also typically contain a zinc element to optimize the deposition process of phosphoric acid on the surface of the item of interest. The use of the bath process is practical for coating a particular type of portion or portion, ie large items whose surfaces are exposed to elements, but the bath process requires that the portion to be treated be disassembled to accommodate the coating.

US Pat. No. 5,540,788 to DeFalco discloses a process for creating an iron-phosphorus surface by forming a conversion surface over an iron substrate by delivering a phosphatizing compound in a lubricating liquid. . This method involves the formation of a conversion surface to create an iron / phosphate surface on the finished machine engine. The composition may be introduced into the run engine through lubricating oil. The disclosed composition comprises a source of phosphoric acid, an alkali metal hydroxide and a source of reactive NH ₂ groups. In particular, the source of reactive NH ₂ group is to prepare a reactive NH ₂ group as a result of the exothermic reaction (exothermic reaction) of the described high. Testing indicates that the same compound, which acts as a source of reactive NH ₂ groups in the exothermic reaction, does not produce reactive NH ₂ groups when following different reaction pathways under different physical conditions. Reactive NH ₂ groups made in the DeFalco patent are best described as phosphamids. This specific chemistry results from the highly exothermic reaction described in the DeFalco patent. It is also noted that physical conditions with high pH result in the production of free ammonia. As the phosphamide circulates with the lubrication medium in the engine, a specific phosphate-iron conversion surface was created for this composition.

Various forms of phosphate-containing materials have been used to produce the desired conversion surfaces on iron as well as non-ferrous metals, each producing a specific surface with unique properties. Most efforts have focused on the deposition of phosphorus-containing coatings on iron substrates and include the use of zinc. When contacted with a metal substrate or metal part, it would be advantageous to create a cost-effective composition that produces a phosphate-metal conversion surface. It would be advantageous if such a composition was useful for the conversion of the iron surface. It would be advantageous if such a composition was useful for the conversion of non-ferrous surfaces that could form a conversion surface. It would be particularly advantageous if such a composition was useful for the conversion of aluminum surfaces comprising aluminum alloys. It would be advantageous to create a conversion surface that is resistant to corrosion and has a high lubricity coefficient even when dry. It would be advantageous to include a method of delivering such a composition without disassembly of the fragments to be coated.

In addition to iron components, there are numerous efforts to produce improved non-iron components, in particular aluminum components. 2-cycle engines commonly found in snow mobiles, lawn mowers, weed-trimmers, mopeds, outboard motors, ATVs, unpacked This effort to create improved aluminum components, such as road bikes, chain saws, and the like, has typically focused on aluminum alloy compositions as a counter to the creation of transition surfaces. For example, unique silicon-aluminum alloy compositions are disclosed in US Pat. No. 6,419,769. Similarly, rare earth elements have been added to aluminum alloys for strength, such as the compositions discussed in US Pat. No. 5,284,532.

Because of typical applications, two-cycle engines are often rarely used. For example, snowmobiles do not run during off-season. This brings additional problems related to condensation and corrosion generation. Corrosion inhibitors are often added to avoid this type of problem.

The aluminum alloy engine contains lubricant for lubricity of the engine. Lubricants are selected to minimize wear of high film strength. This prevents metal-to-metal contact and provides protection against piston scuffing. When the operating temperature is high, the two-cycle motor loses power and torque. Aluminum pistons expand from heat and cause an increase in friction. Various proprietary lubricants have been introduced on the market to improve working performance at high operating temperatures. The ASTM D-4863 two-cycle motor lubricity test measures torque output at 350 ° C. (662 ° F.), which is the basis for working performance.

The field of lubrication technology is characterized by constant research for improved lubricants and additives. Additives essential for the satisfactory working performance of lubricants for all types of modern engines play many roles, including cleaning power, antioxidant properties, and suspension of contaminants. In an effort to improve lubricity, various synthetic oils and various additives have been studied. Additives have also been proposed to reduce wear. One embodiment is US Pat. No. 6,242,394, which discloses a two-stroke cycle lubricant. U. S. Patent No. 6,172, 013 discloses lubricating oil compositions having enhanced coefficient of friction and wear through the use of additives of molybdenum and aliphatic or aromatic dicarboxylic acids. Additives of glyoxylic acid and phenols are known. For example, US Pat. No. 5,281,346 to Adams discloses a two-cycle engine lubricant comprising alkaline earth metal salts or alkali salts of carboxylic aromatic acids.

Various forms of phosphoric acid-containing materials have been studied in order to produce the desired lubricants or surfaces for which each phosphoric acid-containing material produces specific surface compositions having unique properties. Most efforts have focused on the deposition of phosphorus-containing coatings on substrates and include the use of zinc. It would be advantageous to create a cost-effective composition that produces a phosphate-metal conversion surface on a non-ferrous surface. It would be advantageous to create a phosphate-metal conversion surface on an aluminum alloy engine. It would be advantageous if this conversion surface could be created on an engine or component during operation. It would be advantageous to create a conversion surface on the aluminum alloy engine that improves dry lubricity, efficiency, strength and / or emission control. It would be advantageous to include a method of delivering such a composition to the portion to be converted without disassembly of the fragment to be coated. It would be advantageous to produce compositions and methods that do not require zinc.

Summary of the Invention

The present invention includes compositions and methods useful for creating phosphorus-containing conversion surfaces on metal components. The compositions of the present invention are useful for creating thin layers on metal surfaces.

The present invention includes phosphorus-containing solutions containing [Y] H ₂ PO ₄ , [Y] ₂ HPO ₄ , and water or other solvents as components of an intermediate solution, wherein Y is a cation. [Y] H ₂ PO ₄ , [Y] ₂ HPO ₄ as well as other salts discussed herein are also referred to as salt components. The cationic portion of the salt component may be any cation with potassium being the preferred cation. In this case, preferred components would be KH ₂ PO ₄ , K ₂ HP0 ₄ , and water. The intermediate solution is mixed with the carrier liquid. Carrier liquids are liquids capable of maintaining salts at least partially dispersed in the carrier liquid. The water or other solvent used in the medium solution is then mostly removed so that the salt remains at least partially dispersed and / or partially dissolved in the carrier liquid to produce a phosphorus-containing solution. The resulting phosphorus-containing solution may produce a phosphate-metal layer on the metal substrate when placed in contact with the metal substrate.

Preferred cation groups for salts are alkali metals or group 1A elements. Although orthophosphoric acid has been described, the present invention also includes pyrophosphoric acid, which is a condensed analog, a derivative of orthophosphoric acid, and is equivalent to orthophosphoric acid. Through the process of condensing orthophosphoric acid with pyrophosphoric acid, it is known that PO ₄ ^3- becomes P ₂ O ₇ ^2- or other condensed phosphoric acid. Therefore [Y] H ₂ PO ₄ , [Y] ₂ HPO ₄ and [NH ₄ ] ₂ HP0 ₄ are precursors to pyrophosphoric acid. The use of the pyrophosphate form is therefore included within the definition of the orthophosphoric acid form, which can be expressed in [Y] H ₂ P0 ₄ , [Y] ₂ HP0 ₄ and [NH ₄ ] ₂ HP0 ₄ and valuable forms.

Advantageously, the phosphorus-containing solution is essentially free of zinc. Some zinc may be present in solution, but, for example, when zinc is present in the raw material, zinc is not added or present in an amount beneficial for plating. The phosphorus-containing solution is therefore considered to be essentially zinc free. Advantageously, the solution is also substantially free of halogen.

Another preferred embodiment of the phosphorus-containing solution includes the addition of [NR ₄ ] ₂ HPO ₄ to a mediated solution of [Y] H ₂ PO ₄ , [Y] ₂ HPO ₄ , and water or another solvent. R in [NR ₄ ] can be an alkyl group, hydrogen, or a combination of both. Therefore it includes ammonium as well as amine phosphoric acid. When the solution is prepared using an ammonium compound or an amine compound, the nitrogen in the solution is essentially all in the form of ammonium or amine ions. At best, there is a negligible amount of free ammonia, so the solution is substantially free of ammonia.

Another embodiment includes the addition of [X] C ₂ H ₃ 0 ₂ , wherein C ₂ H ₃ 0 ₂ ^- ions are an acetate group, so that the intermediate solution is at least [Y] H ₂ P0 ₄ , [Y] ₂ HP0 ₄ , [X] C ₂ H ₃ 0 ₂ and water or other solvents. Preferred embodiments include X as NH ₄ or K or other group IA element. [NR ₄ ] ₂ HPO ₄ , wherein R is hydrogen, an alkyl group, or a combination of both, may also be added to this mixture. This intermediate solution is combined with a carrier liquid and water or other solvents are mostly removed to produce a phosphorus-containing solution. Although volatility is not a required property, preferably solvents such as alcohols have sufficient volatility to be removed from the intermediate solution mixed with the carrier liquid through the addition of heat. When a phosphorus-containing solution is prepared using the compound, ammonium compounds are defined as such compounds containing NH _x groups, and the nitrogen in the phosphorus-containing solution is essentially all in the form of ammonium ions. Amine ions are also included here. At best there is a negligible amount of free ammonia. Moreover, the mixture is advantageously produced without producing excess heat, ie no exothermic reaction is carried out.

In a preferred embodiment, the phosphorus-containing solution has a pH of about 6.0 to 8.0.

The phosphorus-containing solution of the present invention can be used in various types of environments, such as aqueous or hydrophilic environments. In the case of a hydrophilic environment, it is advantageous to include a carrier liquid and a dispersant to promote dispersion in the carrier liquid. The carrier liquid may be a lubricating liquid disposed to be in contact with the metal part or metal substrate, or in a preferred embodiment, the carrier liquid is a separate hydrophilic liquid that can be highly miscible with the lubricating liquid, such as motor oil. One property of the carrier liquid is that the salt of the phosphorus-containing solution is at least partially soluble in the carrier liquid.

In certain circumstances, the carrier liquid is the amount of the target fluid, such as a lubricating liquid. Target liquids are liquids that are considered to be most liquids intended to contact the phosphorus-containing solution with the metal to be treated. The phosphorus-containing solution can be dispersed through the target liquid using physical mixing, such as a high speed shear mixer or other means. In this case, the target liquid functions as a carrier liquid.

The present invention includes a process for creating a conversion surface on a metal part or metal substrate using a phosphorus-containing solution in a system. The system may be as simple as a metal part that may be in contact with the phosphorus-containing solution or may be a composite of a series of parts as in an engine, where the phosphorus-containing solution is in contact with at least the system part. Where the portion is at least partially in contact with the phosphorus-containing solution or the target liquid containing the phosphorus-containing solution, the phosphate-metal layer surface forms a conversion surface or a phosphate-metal layer on the surface of the metal substrate contacted by the phosphorus-containing solution. The branches are formed while producing a converted metal substrate. The amount of phosphorus-containing solution used is an amount effective to produce the conversion surface. Preferred embodiments of the target liquid in contact with the portion include a lubricating liquid or a phosphate bath. The resulting conversion surface as a result of this process has properties and compositions specific to the metals and phosphorus-containing solutions contained within the metal parts. When the metal part comprises iron, a phosphate-iron surface is created on the iron surface. When the metal part comprises aluminum, an aluminum-phosphate surface is created. When the metal contains nickel, a phosphate-nickel surface is produced. Similar results are observed for chromium and molybdenum.

In addition to being useful for ferrous metal components, the present invention includes compositions and methods useful for creating phosphorus-containing conversion surfaces on non-ferrous components, such as aluminum two cycle engines. Useful for generating

One preferred embodiment includes a lubricating composition or lubricant having a substantial amount of oil with lubricating viscosity. The amount of phosphorus-containing solution is added to the oil, thereby producing a lubricating composition that can create a conversion surface over the metal component that is to come into contact with the metal component.

Another embodiment of the present invention includes a method of forming a non-ferrous metal-phosphate conversion surface over a non-ferrous metal component by contacting a non-ferrous metal component in a contacting zone with an active phosphorus solution. The contact zone may be limited to the surface portion of the metal component and may include the entire metal component. Active phosphorus solutions are prepared by mixing phosphorus-containing acids with alkali metal hydroxide salts and ammonium / amine compounds under conditions designed to produce a highly exothermic reaction, thereby preparing an active phosphorus solution. Ammonium / amine compounds contain either ammonium or amines and can interact in an exothermic reaction. Ammonium hydroxide and ammonia paratungstate are two examples of such ammonium.

details

Whereas active phosphorus solutions have been disclosed as useful for preparing transition surfaces on iron, new studies have shown that when the active phosphorus solution is transferred to the surface of aluminum in a suitable carrier, the active phosphorus solution can be used to create a transition surface on aluminum. Indicates.

Many engines are iron, while two-cycle engines tend to be made of aluminum. The present invention is also useful for the generation of conversion surfaces on such engines. The phosphorus-containing solution of the present invention may be introduced into the engine during use through liquid circulation in parts.

An aluminum-phosphate conversion surface is produced on which the aluminum portion or engine is in contact with the phosphorus-containing solution or the active phosphorus solution of the present invention. With a solution of either of these, the conversion surface can be produced in a bath process or in situ. Unlike typical electro-deposition in solution, the phosphorus-containing solution of the present invention does not use zinc. The phosphorus-containing solution can be delivered in contact with the target liquid to create an aluminum conversion surface over the aluminum portion. Examples of preferred target liquids are lubricants in two-cycle aluminum engines as part of motorized vehicles or other devices. The phosphorus-containing solution is combined with the lubricating oil to produce a lubricating composition. A lubricating composition comprising a significant amount of oil with lubricating viscosity and an amount of phosphorus-containing initial solution can create a transition surface over the aluminum portion or metal component. Like the phosphorus-containing solution, the active phosphorus solution is also useful for contacting the active phosphorus solution with an aluminum engine, preferably by contacting through the use of a target liquid, to create a conversion surface over the aluminum portion.

For the lubricating composition, examples of the amount used in the test include an amount of about 0.01% to about 0.5% by weight of phosphorus in the lubricating composition. A preferred embodiment is 0.3% by weight of phosphorus. Increased amounts of phosphorus are of course effective. It is excellent that very cost-effective solutions can be prepared with low weight percent of phosphorus.

Phosphorus-containing solutions are used to create the conversion surface on the engine for the benefit derived from the engine, whereas the process of the present invention is directed to producing the conversion surface using the phosphorus-containing solution of the invention on a metal part or metal substrate. Include. For example, aircraft components are often made of aluminum. Applying the transition surface over the aircraft components can reduce the coefficient of friction. Motorboat engines, lawn mowers, or other devices that include metal motors or metal parts benefit from the conversion surface of the present invention. By creating a cost-effective way of creating a conversion surface, applications for a wide range of devices have become economically viable. This process is also used with solutions that are active on non-ferrous components.

The conversion surface is created as a result of contacting the aluminum alloy of the part or component with the amount of active phosphorus solution or phosphorus-containing solution capable of producing the conversion surface. The conversion surface produced using the phosphorus-containing solution includes aluminum phosphate and aluminum oxide. The addition of the phosphorus-containing solution to the aluminum surface results in the formation of the reaction product of AlPO ₄ , aluminum phosphate, and Al ₂ O ₃ , aluminum oxide as conversion surfaces on the aluminum component. Test runs using infrared and X-ray testing techniques confirm the presence of these species. Other aluminum species are also prepared differently depending on the aluminum alloy composition and side reactions of the aluminum surface.

Example 1:

One embodiment of the preferred formulation includes a phosphorus-containing solution having the following amounts

1.597 mol KH ₂ PO ₄

0.693 mol K ₂ HP0 ₄

0.315 mol [NH ₄ ] ₂ HP0 ₄

And water.

In this example, the identified salts are mixed and dissolved in a sufficient amount of water to at least partially dissolve the salts. The test shown above used 55.6 moles of water. In this case this produces an intermediate solution having a KH ₂ PO ₄ 2.9 mol%, K ₂ HP0 ₄ 1.2% mol, K ₂ HP0 ₄ 0.5% by mole and 95.3 mole% water. The intermediate solution is then mixed with the carrier liquid. The water is then removed from the mixture of the medium solution and the carrier liquid to prepare the phosphorus-containing solution of the present invention. The resulting phosphorus-containing solution of the present invention means that it is substantially dry or free of water because there is a negligible amount of water left in the solution. Preferably the water is removed to a level of about 0.1 wt% of the phosphorus-containing solution. While more water may be left without changing the functionality of the phosphorus-containing solution, it is noted that 0.1 wt% was chosen as the preferred product specification.

Phosphorus-containing solutions with K or other cations of 0.16 to 16 mol% were evaluated. Solutions outside this range will also be effective, although the cost effectiveness or degree of efficiency may vary.

The pH of the phosphorus-containing solution can be controlled through manipulation of the component proportions. By manipulating the resulting H ₂ PO ^4- and HP0 ₄ ^2- ion ratios, the phosphorus-containing solution can be produced in the preferred pH range of about 6.0 to about 8.0. For example, the ratio for pH 6 is approximately 15.8. The ratio for pH 8 is about 0.0158. Although the entire range was neutral, the test results were controlled for pH 7, and the results were desirable. Through simulations, the following amounts are considered to achieve the indicated pH using the ratio as the only means of manipulating the pH.

Example 2:

Preparation of the formulation includes dissolving KH ₂ PO ₄ , K ₂ HP0 ₄ and Kacetate salts in water. No ammonium salt is used in this example, so the final formulation will not contain ammonia.

The procedure includes adding 51 lbs of deionized water, 17.6 lbs of KH ₂ PO ₄ , 14.2 lbs of K ₂ HP0 _4, and 2.2 lbs of K acetate to two 5-gallon plastic barrels. Thereafter additional 16.4 lbs of water was added. The salt was added to the water with rapid mechanical stirring and the mixture was heated after all the salt was added. Dissolution of KH ₂ PO ₄ was slightly endothermic and the temperature of the batch was dropped by 4-5 ° C. Although no complete dissolution is necessary, this experiment involved heating the mixture to 40 ° C. to dissolve the remaining salts. Alternatively, if complete dissolution is needed, additional water may be added. The pH after complete dissolution was in the target range of 7.0-7.1, so no adjustment of pH such as the addition of KOH or acetic acid. The P value produced after the final dilution was approximately 65,000 ppm and therefore no salt crystallized from the solution.

Examples 3-5 5: The following mediated mixtures were formed and tested:

Example 3

Example 4

Example 5

In this intermediate mixture, KH ₂ P0 ₄ is 38 to 55 mol% of the salt. K ₂ HP0 ₄ ranged from 24 to 35 mole percent of salt. The salt was diluted with water so that the number of moles of phosphorus (P) per liter of medium solution was approximately 2.61 mol / L. This intermediate solution was mixed with the carrier liquid. Phosphorus-containing solutions made at much lower concentrations of phosphorus have also been found to be effective.

Example 6:

1.597 mol KH ₂ PO ₄

0.693 mol K ₂ HP0 ₄

0.315 mol [NH ₄ ] ₂ HPO ₄

0.289 mol [NH ₄ ] C ₂ H ₃ 0 ₂

And water.

[NH ₄ ] C ₂ H ₃ 0 ₂ may also be called [NH ₄ ] acetic acid.

In a preferred embodiment, KH ₂ PO ₄ , K ₂ HP0 ₄ , [NH ₄ ] ₂ HPO ₄ and water are produced as an intermediate solution added to the purified oil carrier liquid and mixed with a dispersant to produce a phosphorus-containing solution. Representative dispersants include alkenyl succinimides or similar types of dispersants including the already distributed product TFA 4690C. In a preferred embodiment, a dispersant having a total base number of 30 to 160 on an oil-free basis is used. While the purified oil carrier liquid ranges from 88 to 92 wt% of the resulting mixture, the phosphorus-containing solution preferably ranges from approximately 8 to 12 wt% of the intermediate solution. In a preferred embodiment the medium solution is added at approximately 10 wt% of the purified oil carrier liquid. The resulting mixture is heated to remove a significant amount of water. The resulting mixture exhibits properties that can be described as colloids or emulsions. When the medium mixture is mixed with lubricating oil, the effective amount of phosphorus in the phosphorus-containing solution can be very diluted and still remains effective. One of the preferred embodiments is 0.3 wt% phosphorus in the intermediate solution. When added to lubricating oils, the phosphorus content can fall in the range of 5-100 ppb and is still effective. The preferred range of phosphorus in the phosphorus-containing solution is 300-1250 ppm. More preferred range of phosphorus is 300-600 ppm. Particularly preferred range of phosphorus is 300-400 ppm. As seen in the previous embodiment, larger amounts are also effective.

An example of another embodiment of the phosphorus-containing solution includes mixing about 2.6 molar (M) orthophosphoric acid, having pH 7 at ambient temperature, with an alkali metal and an ammonium cation. The measured volume of this aqueous phosphorus-containing solution is suspended in an oil-dispersant mixture from which most of the water is thermally removed and diluted to about 0.3 wt% P. Advantageously, while the engine is running, the phosphorus-containing solution can contact the metal parts without disassembling the engine.

Laboratory tests with phosphorus-containing solutions of KH ₂ PO ₄ , K ₂ HP0 ₄ , [NH ₄ ] ₂ HPO ₄ and water as additives show major improvements. Sodium was also evaluated for use as cations in these formulations. Group IA metals are preferred cations. Other cations can include organic ammonium. Factors involved in the selection of cations include commercial cost and / or corrosion resistance.

Laboratory measurements revealed the nature of the surface layer. Application of the phosphorus-containing solution to 1018 carbon steel at 180 ° F involved a series of analytical tests. Optical microscopy (20X) clearly showed a fairly uniform surface layer from the application of the phosphorus-containing solution of the invention to carbon steel. After treating the phosphorus-containing solution in the oil-based mixture, the electron scanning microscope (SEM) of the steel surface shows a relatively smooth layer. Surface analytical instrument measurements in the art have shown that a thin surface conversion layer in the range of 15-80 Hz, depending on conditions and concentrations, is formed. This layer is a variable composition and contains Fe, O, P, N, and K. The layer is thought to be formed from the reaction of the phosphate species in the mixture with the oxidized surface of the metal (Fe), initially about 25 mm thick. The surface ammonium produced from this chemical reaction to produce the conversion layer is obtained from simple FeP0 ₄ to NH ₄ Fe ₂ [PO ₄ ] ₂ , K ₃ Fe ₃ [PO ₄ ] ₄ xH ₂ 0, NH ₄ Fe ₃ depending on the operating conditions. [H ₂ PO ₄ ] ₆ [HPO ₄ ] ₂ .xH ₂ O, KFe ₂ [HPO ₄ ] ₂ [PO ₄ ], and related ammonium, to more complex phosphoric acid. Coordination of the phosphate structure with respect to the surface metal (Fe) ions of the surface layer is believed to be based on the stability of such surface ammonium.

Various oils of lubricating viscosity include natural and synthetic lubricants and mixtures thereof. Such lubricants include crankcase lubricants for spark-ignition and compression-ignition internal combustion engines, including automotive and truck engines, two-cycle engines, aircraft piston engines, marine and rail diesel engines, and the like. They may also be used in gas engines, stationary power engines and turbines. Automatic delivery liquids, transaxle lubricants, gear lubricants, metal-working lubricants, hydraulic liquids and other lubricants and grease compositions also benefit from the combination of the compositions of the present invention. Can be.

Mixtures of phosphoric acid, alkali metal hydroxides and sources of reactive NH ₂ groups are described in US Pat. No. 5,540,788, which is hereby incorporated by reference. Such mixtures, referred to as phosphamid mixtures, have been disclosed for use in the production of iron-phosphate conversion surfaces. The process of producing the phosphamide mixture is not by dissolution but by chemical reaction. The phosphamide mixture is achieved as a result of the highly exothermic reaction resulting in the production of phosphamide. Such active phosphorus solutions such as those used for the production of aluminum conversion surfaces are an improvement in the specification relating to phosphamide and its use.

Phosphamide mixtures as disclosed herein continue to be useful and are the subject of further development. Exothermic reactions under certain circumstances and the preparation of free ammonia at elevated pH are two properties of phosphamide preparation that may be considered less desirable. The phosphorus-containing solution of the present invention is not only free from the consequences and complexity of producing highly exothermic reactions, but is also involved in the preparation of free ammonia and maintaining a pH in the range of approximately 6 to 8, or maintaining a pH below the level at which ammonia is formed No problem.

Testing of the active phosphorus solution indicates that the active phosphorus solution interacts with the non-ferrous metal to produce a conversion surface. Representative non-ferrous metals discussed above are aluminum. The active phosphorus solution produces a phosphorus-aluminum converting surface when contacted with aluminum. Other non-ferrous metals that can produce a conversion surface also interact with the active phosphorus solution.

Although the present invention has been shown and described in only a few forms, it is obvious to those skilled in the art that the present invention is not limited thereto and various changes may be made without departing from the scope of the present invention. For example, the transition surface on the aluminum and iron portions has been discussed in detail. The use of phosphorus-containing solutions or active phosphorus solutions on other metals or metal parts is also included within this invention. Alloys are also included in the discussion of metals.

Claims (33)

Phosphorus-containing solution comprising a mixture of a salt and a carrier liquid comprising: [Y] H ₂ P0 ₄ ; And [Y] ₂ HP0 ₄ , where [Y] is a cation, The carrier liquid may maintain the salt in at least partially dispersed state in the carrier liquid, wherein the phosphorus-containing solution is disposed on the metal substrate when the phosphor-containing solution is placed in contact with a metal substrate. A phosphoric acid-metal layer can be produced, wherein the phosphorus-containing solution is essentially zinc free and the mixture for forming the phosphorus-containing solution is mixed in the absence of a highly exothermic reaction. The phosphorus-containing solution of claim 1 further comprising [NR ₄ ] ₂ HP0 ₄ and R is selected from the group consisting of hydrogen, alkyl groups and combinations thereof. The phosphorus-containing solution of claim 1, wherein substantially free ammonia is free. The phosphorus-containing solution of claim ₁ , further comprising [X] C ₂ H ₃ 0 ₂ , wherein C ₂ H ₃ 0 ₂ is an acetate group and [X] is a cation. The phosphorus-containing solution of claim 4 wherein [X] is selected from the group consisting of potassium, NH ₄ and combinations thereof. The phosphorus-containing solution of any one of the preceding claims wherein the pH of the phosphorus-containing solution is between 6.0 and 8.0. The phosphorus-containing solution of any one of the preceding claims wherein Y in [Y] H ₂ P0 ₄ is potassium. The phosphorus-containing solution of claim 1 wherein Y in [Y] ₂ HP0 ₄ is potassium. The phosphorus-containing solution of any one of the preceding claims wherein Y in [Y] H ₂ PO ₄ and [Y] ₂ HP0 ₄ is selected from alkali metals. The phosphorus-containing solution of any one of the preceding claims further comprising a dispersant. The phosphorus-containing solution of any one of the preceding claims further comprising a target fluid capable of bringing the phosphorus-containing solution into contact with a metal. 12. The phosphorus-containing solution of claim 11 wherein the target liquid is a lubricating fluid. The phosphorus-containing solution of claim 1 wherein the metal substrate constitutes at least part of the engine. The process includes adding the amount of the phosphorus-containing solution of claim 1 to a target liquid effective to produce a phosphate-metal layer, wherein the target liquid in combination with the phosphorus-containing solution is brought into contact with the metal substrate and placed on the metal substrate. Generating a phosphoric acid-metal layer on the metal substrate, wherein the phosphoric acid-metal layer is formed and the metal substrate is at least partially in contact with the target liquid. The phosphorus-containing solution of claim 14 further comprising [NR ₄ ] ₂ HPO ₄ , wherein R is selected from the group consisting of hydrogen, alkyl groups, and combinations thereof. The phosphorus-containing solution of claim 14 or 15, further comprising NH ₄ C ₂ H ₃ 0 ₂ , wherein C ₂ H ₃ 0 ₂ is an acetate group.  The phosphorus-containing solution of claim 16 wherein the pH of the phosphorus-containing solution is between 6.0 and 8.0. 18. The phosphorus-containing solution of any of claims 14, 15, 16 or 17 wherein Y in [Y] H ₂ P0 ₄ in the phosphorus-containing solution is potassium. 19. The phosphorus-containing solution of any of claims 14, 15, 16, 17 or 18 wherein Y in [Y] ₂ HPO ₄ in the phosphorus-containing solution is potassium. 20. The phosphorus of any one of claims 14, 15, 16, 17, 18 or 19 wherein the target fluid is selected from the group consisting of lubricating liquid or phosphating bath. Containing solution. A converted metal substrate comprising a phosphate-metal layer produced by the process of claim 14 to form a conversion surface on the metal substrate. 22. The converted metal substrate of claim 21 wherein the metal substrate comprises iron. The converted metal substrate of claim 21, wherein the metal substrate comprises a non-ferrous metal. 24. The converted metal substrate of claim 23 wherein the non-ferrous metal is aluminum. 24. The converted metal substrate of claim 20, 21, 22 or 23, wherein the metal substrate is at least an engine part. A lubricating composition comprising a substantial amount of oil having lubricating viscosity and lubricating viscosity, and an amount of the phosphorus-containing solution of claim 1 capable of producing a phosphate-metal layer on the metal component in contact with said metal component. Phosphorus is present in the lubricating composition in an amount of 300 ppm to 1250 ppm. A method of lubricating an internal combustion engine comprising supplying the lubricating composition of claim 26 to the engine. A method of forming a non-ferrous metal-phosphate conversion surface on a non-ferrous metal component, comprising the following steps: Preparing a solution that is an active phosphorus solution by mixing a phosphorus-containing acid with an alkali metal hydroxide salt and an ammonium / amine compound to produce an exothermic reaction, thereby preparing an active phosphorus-solution;  Contacting a non-ferrous metal component with the active phosphorus solution in a contact zone above the non-ferrous metal component to form a non-ferrous metal-phosphate conversion surface over the contact zone. . 30. The method of claim 29, wherein the non-ferrous metal component comprises aluminum.  31. The method of any one of claims 29 or 30, wherein the non-ferrous metal component constitutes at least part of the engine. 32. The method of any one of claims 29, 30 or 31, wherein the active phosphorus solution is delivered in contact with the non-ferrous metal in a lubricating environment using a lubricating liquid. Phosphoric acid-metal layer for aluminum components whose surface includes: Aluminum phosphate; And Aluminum oxide, which forms a phosphate-metal layer over aluminum oxide, aluminum phosphate, and an aluminum component, the phosphate-metal layer formed as a result of contacting the aluminum component with the phosphorus-containing solution of claim 1 capable of producing a phosphate-metal layer. .