IMPROVEMENTS IN OR RELATING TO THE FORMATION OF PROFILED CERAMIC BODIES

Abstract: A profiled body of silicon nitride and aluminium nitride dipped in a silica solution such that the silica infiltrates the pores of the body. This silica, together with unconverted si­ lica present in the body, reacts with the aluminium nitride when the body is subsequently fired at around 1800°C in a controlled atmosphere to form sialon. As all the silica is uti­ lised in the reaction, a sialon is formed which can retain its strength up to around 100,000 p.s.i. and at temperatures above 1000°C. Alternatively. the body is infiltrated with alumina to form sialon when fired to at least 1800°C in a controlled at­ mosphere.

Description: Improvements in or relating to the Formation of Profiled Ceramic Bodies This invention is concerned with improvements in or relating to the production of ceramic materials and particularly to the formation of profiled ceramic bodies. The invention is particularly concerned with the formation of such bodies which have high strength characteristics and the ability to withstand high temperatures, such bodies being advantageously used in the production of military aircraft engines for the aerospace industry. Silicon nitride is a conventional engineering ceramic material used for the manufacture of profiled bodies, but reaction bonded silicon nitride normally has strength characteristics of 30,000 - 40,000 p.s.i., whereas, in the desired applications, ceramic materials are required having strength characteristics of around 100,000 p.s.i.. Conventionally, to improve the strength characteristics, hot pressing of the silicon nitride is carried out, but this is a time consuming and expensive method which is thus undesiroble, and the strength of the material reduces at around 1,0000C. The reduction in strength of hot pressed material at temperatures of much above 1,000at is due to the presence of sintering aides which react with silica, in the silicon nitride, to form low melting silicates. Alternatively, to provide a high strength material, it has been proposed to combine aluminium nitride and/or alumina with the silicon nitride to form a material now known as "sialon. However glass ca still be formed at the grain boundaries in sialon and therefore, although the sialon material has the required high strength characteristics, it does not have the required high temperature characteristics when so formed. Further, conventional engineering ceramics have intolerable shrinkage levels when injection moulded and thus bodies profiled to high accuracy level cannot be obtained. Hereinafter the term "high strength characteristics is to be interpreted as the property Qf a material enabling the material to retain its strength up to around 100,000 p.s.i., and the term "high temperature characteristics" is-to be interpreted as the property of a material enabling the material to retain its strength at temperatures above 1,0000C. According to one aspect of the present invention there is provided a method of producing a ceramic material having high strength characteristics and high temperature characteristics, the method comprising the steps of combining compatible amounts of silica and aluminium nitride, and firing the combination at a temperature of at least 18000C in a controlled atmosphere. According to another aspect of the present invention there is provided a method of forming a profiled body of a ceramic material having high strength characteristics and high temperature characteristics as hereinbefore defined) the method comprising the steps of mixing silicon with a predetermined quantity of aluminium nitride in powdered form, subjecting the mix to injection moulding so as to form the profiled body, converting the silicon to silicon nitride, introducing a material to voids created in the silicon nitride, and firing the profiled body, whereby reaction of the profiled body with the introduced material and silica which is inherent at boundaries in the formed silicon nitride forms a body having to the high strength characteristics free of unconverted silica to prevent strength loss at high temperatures. Further the invention provides a method of forming a profiled body of a ceramic material having high.strength characteristics and high temperature characteristics as hereinbefore defined, the method comprising the steps of mixing in silicon with a predetermined quantity of aluminium in powered form, subjecting the mix to injection moulding so as to form the profiled body, converting the silicon to silicon nitride and the aluminium to aluminium nitride, introdu cing a material to voids created in the silicon nitride and firing the profiled body, whereby reaction of the profiled body with the introduced material and silica which is inherent at boundaries in the formed silicon nitride forms a body having the high strength characteristics free of unconverted silica to prevent strength loss at high temperatures. Preferably silica is introduced into the voids in the silicon nitride by dipping the profiled body in a silica solution. Alternatively the profiled body may be internally oxidised so as to fill the voids with silica from the silicon nitride. An embodiment of the present invention will now be described by way of example only. In the aerospace industry, high accuracy profiled bodies are required, particularly in military engines, and cores of ceramic material used in the production of the profiled bodies accordingly require a high accuracy profile. It is necessary for such ceramic materials to have high strength characteristics and also high temperature characteristics. To produce such a body, a predetermined amount of aluminium nitride in powder form is firstly milled with a silicon powder and a suitable binMeqrtrto moke a "dough" suitable for injection moulding. The mix is then injection moulded so as to form a profiled body and organic materials in the body such as the binder are then burnt out. The body is subsequently placed in a furnace where nitrogen is passed over the body in a conventional manner to convert the silicon to silicon nitride. The latter material when so formed is formed with pores or voids which occupy around 20% of the volume of the material. The silicon nitride so formed has also present some coherent silica. The profiled body is then dipped in a silica solution such that the silica in solution can infiltrate into the pores. The addition of the silica reduces the like-lihood of shrinkage of the body. The infiltrated silica, as well as the unconverted silica present in the body, reacts with the aluminium nitride when the body is subsequently fired at high temperature, for example around 18000C, in a controlled atmosphere to form sialon. This sialon reacts with the silicon nitride to form a 'dilute" homogeneous sialon which has the desired high strength characteristics. As the unconverted silica has been utilised in this reaction there is no silica left availoble at grain boundaries to form silicates or glasses which would otherwise weaken the material at high temperatures. Any alumina which may be associated with the aluminium nitride as an oxidotion or hydrolysis product, can be compensated for by slightly altering the ratio of the reactants. In this way all reactants are incorporated as a sialon with minimum shrinkage. In a modification of this method, the profiled body moy be internally oxidised so as to fill the void with silica from the silicon nitride. The body may, for example, be infiltrated with a proprietary alumina sol, being then dried and fired to at least 18000C in a controlled atmosphere. Alternatively, the silicon nitride is infiltrated with an aqueous solution of aluminium sulphate. Then before or after drying, the body is treated in ammonia solution so that aluminium hydroxide is precipitated in the pores of the body. Subsequent heat treatment decomposes the hydroxide to aluminium oxide. The body is then fired to at least 18000C in a controlled atmosphere to form a sialon. There is thus provided a method of forming an engineering ceramic having high strength characteristics and high temperature characteristics without the requirement of the time consuming and expensive method of hot pressing silicon nitride and without the inherent disadvantages of combining silicon nitride with aluminium nitride. In a variation of the method, aluminium powder can be milled in the first stage with the silicon powder and the aluminium converted to aluminium nitride simultaneously as the silicon is converted to silicon nitride in the nitriding furnace. Various modifications may be made without departing from the invention.

Claims: 1ajns 1. A method of forming a profiled body of a ceramic material hovin3 high strength characteristics and high temperature charac- teristics os hereinbefore defined, characterised in that the method comprises the steps of mixing silicon with a predetermined quantity of aluminium nitride in powdered form, subjecting the mix to injection moulding so as to form the profiled body, converting the silicon to silicon nitride, introducing a material to voids created in the silicon nitride, and firing the profiled body, whereby reaction of the profiled body and the introduced material and silica which is inherent at boundaries in the formed silicon nitride forms a body having the high strength characteristics free of unconverted silica to prevent strength loss at high temperature. A A-method of forming a profiled body of a ceramic material hoving hich strength characteristics and high temperature charact eritics as hereinbefore defined, characterised in that the method comprises the steps of mixing silicon with a predetermined quantity of aluminium in powdered form, subjecting the mix to injection moulding so as to form the profiled body, converting the silicon to silicon nitride and the aluminium to aluminium nitride, introducing the material to voids created in the silicon nitride, ond firing the profiled body, whereby reaction of the profiled body with the introduced material and silica which is inherent at boundaries in the formed silicon nitride forms a body having the high strength coracteristics free of unconverted silica to prevent strength loss at high temperatures. 3. A method according to claim 1 or 2, characterised in that the introduced material is silica with which the aluminium nitride reacts. 4. A method according to claim 1 or 2, characterised in that the introduced material is alumina. 5. A method according to claim 4, characterised in that the alumina is introduced in the form of an alumina sol. 6. A method according to claim 4, characterised in that the alumina is introduced by adding aluminium sulphate, the body being treated in ammonia solution to precipitate aluminium hydroxide in the voids and then being heated to decompose the aluminium hydroxide to aluminium oxide prior to firing. 7. k method according to claim 1 or 2, characterised in that the profiled body is internally oxidised so as to fill the voids with silica from the silicon nitride. 8. A method of producing a ceramic material having high strength characteristics and high temperature characteristics as hereinbefore defined, charocterised in that the method comprises the steps of combining compatible amounts of silica and aluminium nitride, and firing the combination at a temperature of at least 18000C in a controlled atmosphere.

Inventors: WILSON, WILLIAM IAN
Applicants: TRW CERAMICS LIMITED
Application year: 1982
Main classification: C04B35
IPC codes: C04B35, C04B41