WO1990013524A1 - Article faconne ayant une matrice cimentee, ainsi qu'un procede et une composition servant a la preparation de celui-ci - Google Patents

Article faconne ayant une matrice cimentee, ainsi qu'un procede et une composition servant a la preparation de celui-ci Download PDF

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Publication number
WO1990013524A1
WO1990013524A1 PCT/DK1990/000113 DK9000113W WO9013524A1 WO 1990013524 A1 WO1990013524 A1 WO 1990013524A1 DK 9000113 W DK9000113 W DK 9000113W WO 9013524 A1 WO9013524 A1 WO 9013524A1
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Prior art keywords
particles
cement
range
average size
shaped article
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PCT/DK1990/000113
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English (en)
Inventor
Hans Henrik Bache
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Aalborg Portland A/S
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Priority claimed from DK212389A external-priority patent/DK212389D0/da
Application filed by Aalborg Portland A/S filed Critical Aalborg Portland A/S
Publication of WO1990013524A1 publication Critical patent/WO1990013524A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/36—Manufacture of hydraulic cements in general
    • C04B7/48—Clinker treatment
    • C04B7/52—Grinding ; After-treatment of ground cement
    • C04B7/527—Grinding ; After-treatment of ground cement obtaining cements characterised by fineness, e.g. by multi-modal particle size distribution
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/0076—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials characterised by the grain distribution
    • C04B20/008—Micro- or nanosized fillers, e.g. micronised fillers with particle size smaller than that of the hydraulic binder

Definitions

  • the present invention relates to improved inorganic binders comprising a hydraulic cement, substantially inert fine particles, and ultrafine particles, which binders have a low proportion of cement, to mortars and concretes having such binders as a binder matrix, to shaped articles comprising a matrix of such binders, to methods of preparing such articles, and to powder mixes for use in preparing the binders, mortars, concretes or articles.
  • WO 80/00959 "Densified cement/ultrafine particle-based materials” (a paper presented by H.H. Bache at the Second International Conference on Superplasticizers in Concrete, Ottawa, Canada, June 10-12, 1981) and WO 81/03170 disclose a class of cement-based materials, the so- called “DSP materials", the binder matrix of which comprises ultrafine particles (A) such as microsilica particles homogeneously arranged between densely packed particles (B) which are exclusively or predominantly cement particles.
  • A ultrafine particles
  • B densely packed particles
  • the dense and homogeneous structure is made possible by the use of an effective amount of a suitable dispersing agent such as a concrete superplasticizer.
  • the binder is made from Portland cement and
  • WO88/00575 discloses a method for the production of DSP materials in which cements which chemically are especially suitable are selected, or measures are taken to improve DSP materials when using cements which in themselves are chemically less suitable for the purpose.
  • JP 50657/1986 discloses DSP materials in which cement particles of an average size of 10.3 ⁇ m are used together with an inert inorganic powder and a superfine powder, the cement particles being used in proportions as low as 10%, to yield cast specimens which show high strengths.
  • JP 50659/1986 discloses cement-based materials comprising metal particles of a size of 1-100 ⁇ m which may replace up to 95% of the cemen .
  • the invention relates to a shaped article comprising a cement-bound matrix, the matrix comprising
  • cement particles having an average size in the range of 2-7 ⁇ m
  • the amount by volume of the particles B being in the range of 0.01- 0.40 times the total volume of the particles B+C,
  • volume ratio of A based on the total volume of A+B+C being in the range of 0.10-0.40
  • volume concentration of A+B+C in the matrix being at least about 0.55.
  • the invention relates to powder compositions and liquid-containing compositions for producing such an article.
  • the marked improvement in quality obtained by the use of the very fine cement particles in low cement binders of the DSP type containing ultrafine particles is related to transport paths during the solidification of the binder, i.e. the solidification of the dissolved "glue" material from the cement particles:
  • the structures are very dense, with ultrafine particles substantially homogeneously distributed throughout the interstices between the larger inert particles C.
  • the amount of cement available for delivering the "glue” is scarce, this being more pronounced the lower the cement content of the binder.
  • the main reason for the improvement obtained according to the main aspect of the present invention is due to the more effective distribution of the scarce "glue” in the dense particle systems with ultrafine particles A in considerable concentrations, in which the possible pathways for the "glue” are very narrow and limited.
  • the surprising effect observed according to the present invention does not seem to be merely an effect of the evidently better distribution of a finer material in a cement binder; experiments performed with low cement materials without ultrafine particles did not reveal any pronounced beneficial effect of using very fine cement particles.
  • substantially inactive or less active than the particles B with respect to solidification of the matrix means that the material of which the particles C consist is not or is only to a very limited extent capable of delivering the chemical "glue” which "glues” the particles together to form a coherent matrix (by dissolution in the aqueous phase, chemical reactions and precipitation of reaction products).
  • the "glue” is delivered predominantly by the cement particles.
  • average size is meant the particle size at which 50% by weight of the particles are larger than the average size (and 50% by weight are smaller) .
  • ultrafine particles A examples include alumina, calcium carbonate, calcium hydroxide, rice husk ash, metakaolin, oxides such as I2O3, SiU2, zirconium oxide and titanium oxide, and ground and/or sieved fly ash, quartz and slag.
  • microsilica that is, silica rich ultrafine dust obtained as by-product in the production of ferrosilicium or silicon metal.
  • the cement may be any hydraulic cement, that is, a powder binder which hardens by reaction with water to form a product which is durable in water.
  • the most important cements are Portland cement and aluminate cement. Examples of cements are normal Portland cement, high early strength Portland cement, sulfate resistant cement, low- alkali cement, low heat cement, white Portland cement, Portland blast furnace cement, Portland pozzolana cement, Portland fly ash cement, and aluminate cement (high alumina cement).
  • Especially preferred cements are white Portland cement and low-alkali cement.
  • the particles C may be any type of inorganic particle which fulfills the above conditions with respect to particle size and which do not to any substantial extent deliver the "glue" in the matrix formation.
  • types of particles C which may be used are fly ash, fine quartz sand, slag, alumina, calcium carbonate and calcium carbonate- containing minerals such as dolomite and calcite, metakaolin, metal particles such as steel powder, and oxides such as AI2O3, S >2, zirconium oxide and titanium oxide.
  • the particles C may advantageously be sorted, e.g. by sieving, so that the particles have a narrow particle size distribution.
  • Special examples of particles C are especially strong mineral particles, e.g. the strong particles used in WO81/3170, such as calcined bauxite particles.
  • the dispersing agents selected should be able to substantially eliminate locking forces between particles in the mix and should have no negative effect with respect to the quality of the final structure.
  • the dispersing agent is normally a concrete plasticizer, in particular a concrete superplasticizer, also called a water reducing agent or a high performance water reducing agent.
  • Such agents are known to be effective with respect to rendering possible the distribution of ultrafine particles, such as ultrafine silica, between densely packed cement particles.
  • concrete superplasticizers such as a sodium salt of a highly condensed naphthalene sulphonic acid/formaldehyde condensate, of which typically more than 70% consists of molecules containing 7 or more naphthalene nuclei
  • the amount of superplasticizer dry matter used is 0.1-4 percent, calculated on the total weight of the particles A, B and C.
  • An alternative manner of expressing the amount of dispersing agent would be to refer it to the particles A and B solely.
  • the amount of superplasticizer dry matter may be expressed as being 1-4 percent by weight, calculated on the weight of the ultrafine particles A and the cement particles B.
  • the present invention should not be limited to any theory, it is believed that .one of the main reasons for the attainment of the remarkable improvements according to the invention resides in the construction of the binder with the ultrafine particles A arranged densely and homogeneously and effectively bound together by cement delivered by the fine cement particles.
  • This ultrafine system is then protected by a rigid "skeleton" formed by the larger particles, that is, the particles C and possibly to a certain extent the cement particles, this protection conferring toughness and stiffness to the ultrafine structure.
  • the cement particles B are very fine as stated above, and it is also preferred that very small particles C contribute to the building up of the skeleton.
  • the particles C (and preferably the particles B) should be large compared to the ultrafine particles, which means that the particles C (and preferably the particles B) should preferably have an average size of at least 3 times the average size of the particles A, preferably at least 10 times the average size of the particles A, and more preferably at least 100 times the average size of the particles A.
  • the cement particles B, and the particles C have a narrow particle size distribution, e.g. do not have any substantial particle size fraction approaching the size of the ultrafine particles, so that the particles B and C do not interfere with the packing of the particles A.
  • the density of the matrix should be high, as stated above at least a volume density of the particles A+B+C of 0.55. This Is obtained in a manner known per se , by using an effective dispersing agent in a sufficient amount, and, quite generally, by using well-known measures to secure a dense and homogeneous structure, such as careful mixing and securing that the matrix-forming materials are mutually compatible, which may be assessed, e.g., by a flow test as described in the examples.
  • a high density of the binder secures that the particles B and C can arrange themselves so that they are in substantially direct particle-to-particle point contact to promote the formation of strong inter-particle bonds between the particles of the protecting "skeleton".
  • the volume concentration of the particles A+B+C in the matrix is at least 0.60, more preferably at least 0.70, and still more preferably at least 0.75.
  • the content of the cement particles B is in the range from 0.01 to 0.40 by volume, calculated on the volume of the particles B+C.
  • the materials of the invention range from very high strength binders with cement contents in the range of 20-40% by volume, based on the volume of the particles B+C, via strong binders with a cement content in the range of 10-20% by volume, to materials having cement contents in the range from 10% by volume down to extremely low contents such as 6%, 3%, 1.5% and even 1% by volume, based on the volume of the particles B+C.
  • the binder matrix according to the invention will normally be combined with additional bodies, such as sand to make a mortar, or sand and stone to make a concrete, and that mortars or concretes according to the invention can be reinforced using e.g. steel bars, mesh or wire. Also, due to the high quality of the binder, it is very well suited for being reinforced with fine fibres, whiskers, etc.
  • the high strength shaped binder compositions according to the invention are advantageous for use in, e.g., structural concrete, such as for buildings, bridges and roads, because of their beneficial properties such as very high strength, stiffness and durability, low permeability, increased volume stability, reduced creep, reduced hydration shrinkage and drying shrinkage, and reduced heat development during hydration, as compared with conventional high quality concretes.
  • compositions according to the invention may be advantageous for one or more of the same reasons as stated above, and for purposes where a high concentration of particles C is desirable, such as where the particles C are particles conferring wear resistance, the compositions of the invention will be especially advantageous.
  • compositions according to the invention with very low cement contents are of particular interest when the cement content per se should be kept as low as possible, e.g. for low cement castables which are to be converted into ceramic type materials by heating or firing.
  • the compositions according to the invention are advantageous because of high density, reduced sintering contraction, and higher refractoriness, that is, higher working temperatures, due to the reduced cement content.
  • Portland cement such as low alkali cement or white Portland cement, can be used as the cement In low cement castables according to the invention, due to the very low amount of cement necessary according to the present invention.
  • the average size of the cement particles is preferably In the range of 2-5 ⁇ m, often more preferably In the range of 2-3 ⁇ m.
  • the cement particles in addition to being very fine as defined above, have a narrow particle size distribution with the ratio -*90/ D 10 °f at -h e most about 12.
  • DQQ diameter at which 90% by weight of the particles have a smaller diameter
  • D;LO diameter
  • the particle size distribution should be as narrow as possible, and very desirable values D90/D1O ° r - ⁇ e cement particles are in the range of 3-10, in particular 3-7 and more preferred 3-5.
  • the cement particles should preferably have as little content of very fine particles as possible, as the very fine cement particles may disturb the packing of the ultrafine particles A and/or may dissolve completely in the mix water and cause undesired early hardening phenomena which can disturb the attainment of an optimum homogeneity in the fine particle system.
  • the ratio T>_o/V_ of the cement particles is at the most 1.5.
  • cement particles have a narrow particle size distribution as defined above and have a very small content of very fine particles.
  • Such cement particles are easier to incorporate into the mixes with attainment of maximum density, and apart from giving rise to a higher quality of the resulting shaped articles, they also give advantages during the production of the articles, such as a longer pot life and a lower requirement for the amount of dispersing agent.
  • the particles A have an average size in the range of 0.03-1 ⁇ m, in particular an average size of about 0.1-
  • the particles A used in the examples have an average particle size in this range.
  • the particles A are preferably spherical particles.
  • a relatively broad particle size distribution of the particles A will give the most dense packing under ideal conditions, but this may in certain cases be counteracted because of increasing difficulties in the homogeneous arrangement of the particles, the finer the particles are.
  • the particles A comprise two particle size fractions, such as one in the range of 0.5-1 ⁇ m and another one in the range of 0.05-0.1 ⁇ m, preferably with one or both of the fractions being narrowly graded as mentioned above.
  • interesting particles C are particles having an average size in the range of 50-100 ⁇ m, or particles having an average size in the range of 2-40 ⁇ m, in particular 2-20 ⁇ m, e.g. 2-10 ⁇ m and as small as 2-5 ⁇ m. It is especially valuable to have larger particles C which have a narrow size distribution with the ratio of at the most about 10, preferably of at the most about 6.
  • the particles C comprise two fractions with gap grading, one fraction having an average size in the range of 50-100 ⁇ m and the other fraction having an average size In the range of 2-10 ⁇ m. It Is especially preferred that at least one of the particle C fractions has a narrow particle size distribution, the ratio D90/D10 °f t ⁇ e "action having an average size in the range of 50-100 ⁇ m being at the most 4, and/or the ratio D90/D1O o: - - ⁇ e fraction having an average size in the range of 2-10 ⁇ m being at the most about 8. All of these measures contribute to improving the density and quality of the binder and the processing conditions, corresponding to what is explained above.
  • the particles C are substantially spherical.
  • the invention also relates to a powder composition for use in producing a binder matrix according to the invention, or, expressed in another manner, for use in producing a shaped article according to the invention.
  • the powder composition may be one which contains the ultrafine particles, the cement, and the particles C, and optionally sand, and to which water and the dispersing agent are added to form a mix, or it may be one which additionally contains the dispersing agent, and to which only water is to be added to form a mix.
  • the types and amounts of the constituents and, with respect to the particles, their particle sizes and particle size distributions can suitably be adapted in accordance with the above discussion.
  • Special powder compositions according to the invention are compositions which do not contain cement particles B, but which contain the very special combination of particles A and particles C which comprise two particle size fractions with gap grading as explained above, the particles preferably being spherical, in particular where at least one of the particle C fractions has a narrow particle size distribution as explained above.
  • the invention relates to a fluid composition for use in making a shaped article, the fluid composition either comprising all of the essential constituents for making the binder, that is, the particles A, the cement particles B, the particles C, the dispersing agent, and water, or comprising, e.g., the constituents except the cement, or the constituents without the cement and without the dispersing agent, so that the appropriate amount of cement and an adapted amount of dispersing agent is added to form the final mix.
  • the particles C will be the special particles comprising two particle size fractions with gap grading, and optionally with a narrow particle size distribution in one or both fractions.
  • the amount of water should be kept sufficiently low to allow the attainment of the desired particle concentration in the resulting matrix made from the composition.
  • the production of shaped articles according to the present invention may be performed in accordance with normal mixing and casting techniques as known, e.g., for DSP materials, aimed at arranging the particles in a homogeneous and dense system, that is, with sufficient mixing and sufficiently long mixing times to obtain a well saturated homogeneous dense system.
  • DSP materials e.g., for DSP materials
  • Such methods and additional methods which employ pre-mixing of the finest components and subsequent addition of the somewhat larger particles are described in the Examples.
  • it will be preferred that the curing is performed without any initial heating, so as to make it possible for the small amount of cement to diffuse throughout the ultrafine structure before any substantial hardening takes place, but It is also possible to utilize heat curing and other curing regimens known to increase the strength of conventional cement-bound materials.
  • the components of the particle system should be compatible from a chemical and surface chemical point of view, in particular, the particles A, the cement particles, and the dispersing agent should be selected so that they will be compatible with each other.
  • W088/00575 discloses that the cement and the particles A should be selected and/or the mix adapted so that the content of water-soluble alkali in the mix originating from the mineral solids in the mix is at the most 0.30%, calculated as Na2 ⁇ equivalents, relative to the weight of the cement in the mix.
  • a white Portland cement (density 3150 kg/m , Blaine surface 411 m-/kg) Is employed.
  • the grain size distribution of the white Portland cement used in Example 1 is as follows: % ⁇ 50 ⁇ m 99.0
  • the white Portland cement (very fine white cement I) is finely ground, with a Blaine surface of 757 m-/kg, a BET surface of 2950 m ⁇ /kg and the following particle size distribution:
  • the density of the Portland cement used in these examples is 3171 kg/m 3 .
  • the white Portland cement of Examples 6 and 7 has the following chemical composition (% by weight) :
  • Example 8 an aluminous cement (Alcoa CA-14) with a density of 2999 kg/m- and the following chemical composition (% by weight) was employed:
  • the aluminous cement had the following particle size distribution:
  • Example 9 the aluminous cement was finely ground and had the following particle size distribution:
  • Example 13 a finely ground white Portland cement (very fine white cement II) having the following grain size distribution was employed: % ⁇ 50 ⁇ m 98
  • Example 12 an air-classified white Portland cement (obtained by sorting the cement using an air stream) was employed. Substantially all of the particles of the air-classified white Portland cement had a size of between 2 and 10 ⁇ m. ' The particle size distribution was as follows:
  • Fly ash II has the following grain size composition:
  • Example 5 a finely ground fly ash was employed by grinding of the above-mentioned fly ash II. This fine fly ash had a density of 2717 kg/ and a particle size distribution as follows:
  • fly ash used in Examples 10 and 11 corresponds substantially to fly ash III.
  • Example 12 a fly ash with a narrow grain size distribution (obtained by sorting the fly ash using an air stream) was employed.
  • the air-classified fly ash had an average particle size of about 6.5 ⁇ m and the following grain size distribution:
  • Example 3 finely ground quartz with the following grain size distribution is employed:
  • Example 13 a relatively fine sand (Sa ⁇ by sand) having a grain size of 0-0.25 mm and the following grain size distribution was employed:
  • the above mentioned Sasby sand is sieved and the fine fraction (0-0.25 mm) employed.
  • the sieved fine Sseby sand has a density of about 2600 kg/m3 and the following grain size distribution:
  • Microsilica (microsilica II, density 2220 kg/m 3 , specific surface (BET) 21,400 ⁇ r/kg) with the following chemical composition is used:
  • the employed quartz sand and stone (hyperite) had the following characteristics:
  • the particle size distribution for the fine sand was as follows: % ⁇ 0.500 mm 99
  • bauxite is employed instead of sand.
  • the 0-1 mm bauxite fraction has a density of 3.475 g/cm 3 and the following size distribution:
  • the 1-4 mm bauxite fraction has a density of 3.297 g/cm 3 and the following size distribution:
  • Flube is a sodium salt of a highly condensed naphthalene sulphonic acid/formaldehyde condensate, with an estimated powder density, referring to the density when disolved in water, of 1600 kg/m .
  • the water employed was common tap water.
  • Two types of materials were prepared: mortar having a maximum particle size of less than 4 mm and concrete containing particles larger than 4 mm and having a maximum particle size of either 11 mm or 16 mm.
  • the mortar portion was prepared first, after which the stone was added, so that the mixing of the mortar was the same regardless of whether the mortar was used alone or together with the stone to form a concrete.
  • mixing generally was carried out as follows: Mixing of the mortars took place in a 20 1 paddle mixer (for the preparation of mortar samples) or in a 50 1 paddle mixer (Eirich) (for the preparation of mortars to be used in concrete) .
  • the dry materials i.e. all the materials except water, were first mixed for one minute, after which the water was added while the mixer rotated. The addition of water took about 10-20 seconds. Mixing was then continued for 10 minutes (in certain cases somewhat longer).
  • the mortars' consistency was determined by flow table measurements according to the ASTM flow table measurement technique (ASTM C230-83).
  • ASTM flow table measurement technique ASTM C230-83
  • the diameter of a mortar sample is measured first prior to impact and subsequently after impact performed by letting the mortar sample fall a distance of about 12.7 mm 20 times according to the following procedure: the flow table is dried and the mould (height 50 mm) for casting the flow specimen is placed in the center of the table.
  • a layer of mortar, about 25 mm thick, is placed in the mould using a spoon.
  • the layer is stamped 20 times with a stamper.
  • the stamper pressure is adjusted so that the mould is uniformly filled.
  • the mould is filled entirely with mortar and stamped as above (20 times) .
  • the mould should at least be filled.
  • a steel rod with cross-sectional dimensions of 3 x 3 cm was used as a counterweight. After filling, the molds were closed by fastening a lid on the cylinders. The preparation of samples on the 150 cycles/sec. vibrator table was accomplished with vibration under combined static and dynamic pressure, established with a steel cylinder (weight 8 kg) placed on top of the material during vibration. The samples were cast by pouring the mix in 4 to 5 portions over a period of 1 to 2 minutes. After filling, the molds were closed as described above.
  • the cast samples in the sealed molds were placed in water having a temperature of 80°C within 1 to 2 hours after casting.
  • the samples were removed from the hot water after 24 hours and placed (still in the sealed molds) in air having a temperature of 20°C for approximately 24 hours, after which the molds were removed and the samples were kept in air (20°C, approx. 70% relative humidity) until they were tested for strength, which normally occurred within one week.
  • the cast and sealed samples were kept for 24 hours at 20°C (covered by wet towels and sealed in plastic) , after which the molds were removed and the samples were placed in water with a temperature of 20°C for extended hardening. Some of these samples were tested for strength immediately after curing in water. Others were kept for 5 to 7 days at a temperature of 45°C in air before testing for strength.
  • the density of the samples was determined by weighing the samples out of and in water at a temperature of 20 C C, the density of the water being assumed to be 1000 kg/m 3 .
  • the measured values for density were in many cases compared with the density of the materials, calculated on the basis of the mix compositions and the densities of the individual ingredients, under the assumption that the materials were "perfectly" compacted without the presence of voids (air) . These values are referred to as the "theoretical densities".
  • the sound velocity in the materials was determined (for high frequency low energy waves) by measuring the time it took an impulse to travel through the sample (20 cm for cylinders) .
  • the dyn-amic modulus of elasticity may be calculated as follows:
  • E refers to high frequency low energy performance
  • the compressive strength of the materials was determined in oil pressure driven presses, using either a 600 t press or a 500 t press.
  • the applied stresses increased at a constant rate of 0.8 MPa/sec.
  • the degree of packing of dry sand and stone in open containers was determined. The results are given below, in which the upper number is after simple pouring of the dry materials, and the lower number is after vibration on a vibrator table using a vibration of 50 cycles/sec. for about 15 seconds.
  • the sand was packed in a 3 litre container and the stone was packed in a 1 litre container.
  • Air-classified fly ash 12 12.5 6.4 3.15 2.65 4.0 1.2
  • the mortars are referred to according to the cement content by volume based on the content of cement in a mix C-100%, which contains no fly ash.
  • the binders comprised white Portland cement as the active particles, fly ash and microsilica.
  • the data of the materials appear from "Materials and Methods".
  • the average particle size of the cement was 10.5 ⁇ m; the ratio D90/D10 as H-8* an( i the ratio V_Q/V_ was 1.8.
  • the mix compositions were as follows:
  • Samples were prepared in the form of cylinders (diameter 100 mm, height 200 mm) by casting in an open mold using gentle vibration. The procedure for mixing and casting was as described above in "Materials and Methods".
  • Four cylinders were prepared from each type of mortar. The cylinders were hardened in sealed molds for 2 days, the first 24 hours in hot (80°C) water, and then in 20°C air, after which the samples were removed from the molds and kept in air with a temperature of 20°C. Three of the four cylinders from each type of mortar were tested for compressive strength five days after the samples were removed from the molds. The remaining cylinders (one from each type of mortar) were used for supplementary investigations. Immediately following removal from the molds, all cylinders were weighed (in and out of water) and sound velocity through the samples was determined.
  • Mortars according to the invention containing finely ground cement with average particle size 5.4 ⁇ m
  • the mortars were equivalent to the mortars C-12.5% and C-6% used in the Example 1, with the exception that the cement in Example 1 was replaced by a very finely ground cement having an identical chemical composition to that of the cement of the Example 1.
  • the data of this cement appear from "Materials and Methods".
  • the average particle size of the cement was 5.4 ⁇ m; the ratio Do ⁇ /D jfj was 11.4, and the ratio D 10 / D 5 was I* 5 -
  • the samples were hardened at 80°C in sealed forms in water for 24 hours and then at 20°C in sealed forms for 24 hours, followed by 5 days at 20°C in air.
  • a great number of materials are useful as the fine, inactive particles C.
  • One such type of material is ground quartz.
  • a mortar with ground quartz as particles C can be prepared as follows:
  • Mortars may also be prepared according to the following mixes, which contain various materials as the fine, inactive particles C.
  • Mix ref Mix 1 Mix 2 Mix 3 Mix 4
  • Precipitated CaC0 3 average particle size 0.7 ⁇ m, surface area 23 m 2 /g Fine A1 0 3 : average particle size 0.5 ⁇ m, specific surface (BET) 3.5 m 2 /g
  • Calcite filler 98% ⁇ 50 ⁇ m, 59% ⁇ 10 ⁇ m, 16% ⁇ 1 ⁇ m, density
  • a concrete with a fine mortar and a high concentration of irregularly shaped stone (5-11 mm) can be prepared as follows:
  • the fine mortar comprises the same binder material as in Example 2, (C-25%).
  • the mix composition is as follows:
  • Samples are produced as described above in "Materials and Methods" by mixing in a 50 1 paddle blender in a two-step process, i.e. first the mortar is mixed, after which (after addition of the stone) the concrete is mixed.
  • a flow table measurement is performed on the mortar as described above.
  • Cylinders (200 mm x 100 mm diameter) are prepared by casting using a vibration of 150 cycles per second with a counterweight, as described above.
  • the mortar was a "standard mortar” with the same sand composition as in Example 1 and with the same volume of binder powder.
  • the water content was in this case about 20% greater.
  • the mix composition was as follows:
  • the total volume (sum of the dry constituent components + water) of the mixes is 35 litres.
  • the mix compositions (in grams) are as follows:
  • a series of cylindrical samples (200 mm x 100 mm in diameter) is prepared by casting using a vibration of 150 cycles per second with a counterweight, as described above.
  • Concrete cylinders using steel powder and bauxite may be prepared as follows:
  • Cylinders (200 mm x 100 mm diameter) are cast, cured at 20 C C and 100% relative humidity for 48 hours and removed from the molds.
  • the cylinders are cast from the following mix: White cement* 7724 g
  • the steel powder has a density of 7628 kg/m 3 and the following particle size distribution:
  • a mortar was prepared having a relative mix compositions identical to mix C-6% of Example 6, with the exception that the white Portland cement was replaced by a refractory high alumina cement (Alcoa CA-14) on a volume for volume basis.
  • the mix composition was as follows: C-6%
  • the samples were then submerged in water at 20°C and cured until 28 days had elapsed since initial casting. After 28 days, 3 samples from each series were removed and the density, sound velocity and dynamic modulus of elasticity were determined. The samples were then dried for 5 days at 45 C C, after which the compressive strength was determined. The results are given below.
  • Example 8 Using the aluminous cement of Example 8 which had been finely ground to give the particle size distribution listed under "Materials and Methods", 18 cylinders (200 mm x 100 mm in diameter) were cast. It was noted that a relatively long mixing time was required before the dry mix acquired a plastic consistency.
  • the composition of the mix was as follows (6% by volume cement, based on cement + fly ash):
  • the cylinders were hardened at 20°C and 100% relative humidity for 24 hours, after which the molds were removed and the density and dynamic modulus of elasticity were determined. The following results were obtained (standard deviations in brackets) :
  • Concrete having an extremely low cement content may be prepared and cast using binders based on very fine white Portland cement, fly ash and microsilica with a volume ratio between cement and cement plus fly ash of 6%, 3% and 1.5%, respectively, and a microsilica content of about 25% based on the total powder volume.
  • the concrete may also contain quartz sand with a size of 0-1 mm and hyperite stone with a size of 5-11 mm.
  • the recipes (weight in g) for the mixes (about 34 1 each) are as follows.
  • the concrete may be prepared as described in Example 4. From each batch, 18 cylinders (20 cm x 10 cm diameter) may be cured as follows.
  • Dense fine material prepared using moderate vibration and pressure compaction
  • the fine components of the fine materials i.e. microsilica (0.2 ⁇ m) , cement (15 ⁇ m) and fly ash (15 ⁇ m) , are uniformly premixed with water and an effective dispersing agent to form a viscous mass with a high particle concentration of about 0.70, corresponding to water saturation just being achieved during the mixing process.
  • “coarse” component of the fine materials i.e. very fine quartz sand (average particle size 80 ⁇ m)
  • the amount of liquid is now too little to saturate the materials during mixing, due to the increase in the amount of particles.
  • the material now obtains an earthy to dry, lumpy to grainy consistency. Small samples of the material are taken and compressed using light to moderate vibration and pressure compaction, whereby the particle system is packed so that the voids are significantly reduced, so that liquid saturation is achieved.
  • fine materials in which the particle concentration (A + B + C, C being the fraction of the fine sand below 100 ⁇ m) is increased from about 0.70 to about 0.82 may be prepared using a process in which 1) the essential homogenous distribution of all of the fine components and the liquid are achieved using fluid-mixing in a saturated state, 2) a relatively homogenous distribution of the coarse components Is achieved by long and thorough intermixing in a powder mass having a plastic to lumpy consistency, and 3) the final, dense particle packing is achieved using vibration and pressure compaction without pressing excess water out of the material, which is required to achieve similar density if the entire mixing process (using more liquid) is to take place at one time in a water saturated condition.
  • the employed fine quartz sand particles has a size in the range of 0-0.125 mm and an average size of 80 ⁇ m.
  • the mix compositions (g) are shown in the following table.
  • composition of the materials without the quartz sand is substantially as given in Example 1 (C-25) , with the exception that the amounts are smaller.
  • Fine materials i.e. cement, fly ash, microsilica and Flube
  • the fine materials are dry-mixed for 1 min. , after which all the water is added and mixing is continued for another 10 min. , followed by further addition of fine sand (see the table with the mix compositions) using a total mixing time of about 45 min.
  • the consistency may be determined visually based on 1) the characteristics of the mixes during mixing, and 2) samples of the mixes, using light to moderate vibration and pressure compaction.
  • small samples of materials with different sand contents in sealed plastic bags may be placed on a vibrator table and vibrated for 20-30 sec. using a metal weight during vibration to press the samples into flat discs with an area of about 10-20 cm 2 .
  • Vibration frequency 50 Hz; acceleration about 100 m/s 2 Weights: about 200 g, 500 g, 8000 g.
  • the following materials are prepared: 1) fine binders with a maximum particle size of about 12 ⁇ m and showing a combination of good fluidity and density, and 2) extremely dense binders prepared by adding fine sand (63-90 ⁇ m) to the fine binders.
  • the binders were tested in a quartz sand mortar.
  • Fly ash air-classified fly ash with a narrow particle distribution and a small particle size (average size 6 ⁇ m and substantially all of the particles between 2 and 12 ⁇ m) , density 2320 kg/m .
  • Microsilica as in Example 1.
  • Sieved fine sand (“Sa ⁇ by sand”) : rounded quartz sand with a particle size between 63 and 90 ⁇ m, density about 2600 kg/m .
  • Quartz sand 0.25-1 mm and 1-4 mm (as in Example 2)
  • the mix compositions (in g) are as follows.
  • the dry materials for the fine mortar were mixed for 1 min. in a Hobart mixer.
  • the water was then added, first 120 g and then gradually to 130 g, and mixing was carried out for 5-10 min.
  • Flow measurements were then made, after which another 5 g of water was added and mixing was carried out for another 5-10 min. , followed by flow measurements for this mix (mix II) .
  • the same precedure was used for mixes III and IV.
  • 750 g of fine sand (63-90 ⁇ m) were then added and mixing was carried out for another 5-10 min., after which 6 cylinders (9 cm x 4.5 cm diameter) were cast using vibration (50 Hz, acceleration about 50-100 m/s 2 ) with a light counterweight.
  • the samples were hardened for about 60 hours in water at 80°C in sealed moulds. The samples were then removed from the moulds and after cooling to 20 ⁇ C density, sound velocity and compressive strength were determined. The results of the flow measurements are given below.
  • the density of 2330 kg/m 3 indicates that the desired extremely dense packing has been achieved, since the theoretical density, under the assumption of 0% air and calculated on the basis of the density of the individual components and the mixing ratio, is 2352 kg/m 3 . This indicates that the material contains only about 1% trapped air.
  • the results of the compressive strength measurements indicate that these are completely unique materials, especially seen in the light of the fact that 1) the ratio B/(C+B) is only 12%, and 2) the mortar was prepared using normal quartz sand and not particularly strong sand.
  • the fine binder of mixes I-IV shows a low maximum particle size of 12 ⁇ m and a very dense packing of the particles A, B, and C, corresponding to a water/cement ratio by weight of about 0.11-0.13 if all particles are calculated as having cement density and ignoring the dispersing agent, in other words in accordance with the calculations in concrete technology.
  • the fine binder also shows a high fluidity, as evidenced by the most dense of the materials being easily castable under vibration, and the other materials being almost self-levelling.
  • the fine binder material shows an excellent performace, as appears from the results obtained with Mix V, where the fine binder was combined with the very narrowly graded fine sand particles. This indicates that the fine binder would be very useful as a binder in e.g. fine components composites, such as composites using 5-15 ⁇ m diameter fibres in high volume concentration, to result in materials of very high quality.
  • the dense binder of mix V shows very excellent properties which would not have been expected to be obtainable in such a material cast with conventional vibration technique.
  • the properties are especially remarkable in view of the fact that the mortar in which the binder is tested is a quartz sand mortar. Still better properties are to be expected when the binder is used in a mortar with strong sand particles such as calcined bauxite.
  • the binder shows a high content, 57% by volume, of particles C, demonstrating the potential of the materials of the present invention in connection with the utilisation of particles C which have special properties, such as magnetic particles or wear resistant particles.
  • Example 2 compared with Example 2, demonstrates the effect of the preferred use of the narrowly graded cement and the narrowly graded fine particles C (in mix V together with narrowly graded larger particles C) , and indicates that excellent materials may be obtained even with very low cement contents in such materials, such as 6%, 3%, and 1% by volume. Finally, the example indicates that still better properties must be expected when these materials are combined, by vibrational compaction, with still higher amounts of the narrowly graded sand, compare the teaching of Example 11.
  • the individual mortars were first mixed using a certain amount of water, after which the amount of water was gradually increased and the consistency and flow behaviour of the mix was observed and measured.
  • the consistency was determined as described in materials and methods, i.e. using the ASTM C230-83 standard for flow table measurements.
  • the materials of the various mixes are also described in the Materials and Methods section.
  • This example shows the effect of replacing fine white Portland cement having a "normal" particle size distribution with a graded (air- classified) fine white Portland cement having a narrow particle size distribution, the water requirement of the mix containing the latter being significantly lower than that of the mix containing the former.

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Abstract

Un article façonné comportant une matrice cimentée ayant une teneur en ciment peu élevée, comportant: A) des particules solides inorganiques qui sont inactives ou sensiblement moins actives que le ciment par rapport à la solidification de la matrice, telles que les particules de silice ultrafines, les particules ayant une taille d'entre 0,002 et 2 νm; B) des particules de ciment ayant une taille moyenne d'entre 2 et 7 νm; C) des particules solides inorganiques qui sont inactives ou sensiblement moins actives que les particules de ciment B par rapport à la solidification de la matrice, telles que des particules de cendres volantes, des particules de bauxite réfractaires, ou des particules métalliques, p. ex des particules d'acier, les particules C ayant une taille moyenne entre 3 et 10 νm, la taille maximum des particules étant de 100 νm; D) un agent dispersant, tel qu'un superplastifiant de ciment (agent réducteur d'eau) en quantité de 0,1 à 4 % par poids de matière sèche, calculé sur le poids total des particules A+B+C, la quantité par volume des particules B étant entre 0,01 et 0,40 fois le volume total des particules B+C, la densité relative en % de A à partir du volume total d'A+B+C étant de 0,10 et 0,40, et la concentration en volume d'A+B+C dans la matrice étant d'au moins environ 0,55, démontre une qualité supérieure, telle qu'une puissance de compression et une durabilité supérieures, en comparaison avec des matières semblables ayant des particules de ciment plus grandes.
PCT/DK1990/000113 1989-05-01 1990-05-01 Article faconne ayant une matrice cimentee, ainsi qu'un procede et une composition servant a la preparation de celui-ci WO1990013524A1 (fr)

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994009339A1 (fr) * 1992-10-15 1994-04-28 Green Clay Aps Article a briser en eclats, composition de moulage et procede de production dudit article
EP0696558A2 (fr) * 1994-08-12 1996-02-14 Dyckerhoff Aktiengesellschaft Mélange de liant à base de ciment ultra-fin procédé pour sa fabrication et dispositif pour la mise en oeuvre du procédé
EP0748782A1 (fr) * 1995-06-13 1996-12-18 Sofitech N.V. Compositions de cimentation et application de ces compositions pour la cimentation des puits pétroliers ou analogues
EP0934915A1 (fr) * 1998-02-06 1999-08-11 Entreprise Quillery & Cie Béton très haute performance, autonivelant, son procédé de preparation et son utilisation
WO2000050362A1 (fr) * 1999-02-22 2000-08-31 Keele University Compositions a base de ciment
FR2813074A1 (fr) * 2000-08-21 2002-02-22 Lafarge Sa Beton a base de liant hydraulique pour la realisation de prefabriques, tuiles, plaques et similaires
WO2002083590A2 (fr) * 2001-04-18 2002-10-24 University College Cardiff Consultants Ltd. Melanges cimentaires
WO2002094735A1 (fr) * 2001-05-23 2002-11-28 Dsm Ip Assets B.V. Procede de fabrication de beton a haute resistance initiale
US6730161B2 (en) * 2001-06-20 2004-05-04 Process Research Ortech, Inc. Treatment of fly ash
FR2859722A1 (fr) * 2003-09-15 2005-03-18 Wheelabrator Allevard Materiau composite a haute resistance a l'abrasion, comprenant de la grenaille a base d'acier et procede de fabrication d'un tel materiau
FR2866330A1 (fr) * 2004-02-13 2005-08-19 Eiffage Tp Beton ultra haute performance et autoplacant, son procede de preparation et son utilisation.
WO2009081277A1 (fr) 2007-12-21 2009-07-02 Lafarge Composition de béton
WO2012023825A2 (fr) 2010-08-19 2012-02-23 Lg Hausys, Ltd. Composition de pâte pour marbre artificiel et procédé de fabrication de marbre artificiel l'utilisant
US8603238B2 (en) 2009-03-24 2013-12-10 Lafarge Concrete with a low clinker content
EP3360854A1 (fr) * 2017-02-10 2018-08-15 Holcim Technology Ltd. Composition de ciment blanc ultra-fin

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EP0010777A1 (fr) * 1978-11-03 1980-05-14 Densit a/s Produit façonné et matériau composite et procédé pour leur fabrication
EP0042935A1 (fr) * 1980-05-01 1982-01-06 Densit A/S Article formé, matériau composite et procédé pour sa préparation
EP0067456A2 (fr) * 1981-06-16 1982-12-22 Dansk Eternit-Fabrik A/S Procédé pour le laminage de matériaux à déformation plastique
US4504320A (en) * 1983-09-26 1985-03-12 Research One Limited Partnership Light-weight cementitious product

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0010777A1 (fr) * 1978-11-03 1980-05-14 Densit a/s Produit façonné et matériau composite et procédé pour leur fabrication
EP0042935A1 (fr) * 1980-05-01 1982-01-06 Densit A/S Article formé, matériau composite et procédé pour sa préparation
EP0067456A2 (fr) * 1981-06-16 1982-12-22 Dansk Eternit-Fabrik A/S Procédé pour le laminage de matériaux à déformation plastique
US4504320A (en) * 1983-09-26 1985-03-12 Research One Limited Partnership Light-weight cementitious product

Cited By (35)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994009339A1 (fr) * 1992-10-15 1994-04-28 Green Clay Aps Article a briser en eclats, composition de moulage et procede de production dudit article
EP0789006A2 (fr) * 1994-08-12 1997-08-13 Dyckerhoff Aktiengesellschaft Mélange sec pour une suspension de ciment, procédé pour sa fabrication et dispositif pour la mise en oeuvre du procédé
EP0696558A2 (fr) * 1994-08-12 1996-02-14 Dyckerhoff Aktiengesellschaft Mélange de liant à base de ciment ultra-fin procédé pour sa fabrication et dispositif pour la mise en oeuvre du procédé
EP0696558A3 (fr) * 1994-08-12 1996-05-22 Dyckerhoff Ag Mélange de liant à base de ciment ultra-fin procédé pour sa fabrication et dispositif pour la mise en oeuvre du procédé
EP0789006A3 (fr) * 1994-08-12 1997-12-03 Dyckerhoff Aktiengesellschaft Mélange sec pour une suspension de ciment, procédé pour sa fabrication et dispositif pour la mise en oeuvre du procédé
EP0748782A1 (fr) * 1995-06-13 1996-12-18 Sofitech N.V. Compositions de cimentation et application de ces compositions pour la cimentation des puits pétroliers ou analogues
FR2735465A1 (fr) * 1995-06-13 1996-12-20 Schlumberger Cie Dowell Compositions de cimentation et application de ces compositions pour la cimentation des puits petroliers ou analogues
US6312515B1 (en) 1995-06-13 2001-11-06 Schlumberger Technology Corporation Cementing compositions and the application of such compositions to cementing oil or analogous wells
EP0934915A1 (fr) * 1998-02-06 1999-08-11 Entreprise Quillery & Cie Béton très haute performance, autonivelant, son procédé de preparation et son utilisation
FR2774683A1 (fr) * 1998-02-06 1999-08-13 Quillery & Cie Entreprise Beton tres haute perfomance, autonivelant, son procede de preparation et son utilisation
WO2000050362A1 (fr) * 1999-02-22 2000-08-31 Keele University Compositions a base de ciment
FR2813074A1 (fr) * 2000-08-21 2002-02-22 Lafarge Sa Beton a base de liant hydraulique pour la realisation de prefabriques, tuiles, plaques et similaires
WO2002016281A1 (fr) * 2000-08-21 2002-02-28 Lafarge S.A. Beton a base de liant hydraulique pour la realisation de prefabriques, tuiles, plaques et similaires.
GB2391010A (en) * 2001-04-18 2004-01-28 Univ Cardiff Cementitious mixtures
GB2391010B (en) * 2001-04-18 2005-07-13 Univ Cardiff Cementitious mixtures and a method of production thereof
WO2002083590A3 (fr) * 2001-04-18 2003-01-03 Univ Cardiff Melanges cimentaires
WO2002083590A2 (fr) * 2001-04-18 2002-10-24 University College Cardiff Consultants Ltd. Melanges cimentaires
WO2002094735A1 (fr) * 2001-05-23 2002-11-28 Dsm Ip Assets B.V. Procede de fabrication de beton a haute resistance initiale
US6730161B2 (en) * 2001-06-20 2004-05-04 Process Research Ortech, Inc. Treatment of fly ash
JP2007505805A (ja) * 2003-09-15 2007-03-15 ウィーラブラトール‐アルバール 鋼基材ショットを含んでなる高耐摩耗性複合材料および該材料の製造方法
FR2859722A1 (fr) * 2003-09-15 2005-03-18 Wheelabrator Allevard Materiau composite a haute resistance a l'abrasion, comprenant de la grenaille a base d'acier et procede de fabrication d'un tel materiau
US7402203B2 (en) 2003-09-15 2008-07-22 Wheelabrator-Allevard High-wearing-resistant composite material comprising steel-based shot and method for producing said material
WO2005040061A1 (fr) * 2003-09-15 2005-05-06 Wheelabrator-Allevard Matériau composite à haute résistance à l'abrasion comprenant de la grenaille à base d'acier et procédé de fabrication d'un tel matériau.
CN1934052B (zh) * 2004-02-13 2011-09-21 埃法日Tp公司 超高性能、自密实的混凝土，其制备方法和用途
FR2866330A1 (fr) * 2004-02-13 2005-08-19 Eiffage Tp Beton ultra haute performance et autoplacant, son procede de preparation et son utilisation.
WO2005077857A2 (fr) * 2004-02-13 2005-08-25 Eiffage Tp Beton ultra haute performance et autoplacant, son procede de preparation et son utilisation
WO2005077857A3 (fr) * 2004-02-13 2006-02-02 Eiffage Tp Beton ultra haute performance et autoplacant, son procede de preparation et son utilisation
US7641731B2 (en) 2004-02-13 2010-01-05 Eiffage Tp Ultrahigh-performance, self-compacting concrete, preparation method thereof and use of same
WO2009081277A1 (fr) 2007-12-21 2009-07-02 Lafarge Composition de béton
US8603238B2 (en) 2009-03-24 2013-12-10 Lafarge Concrete with a low clinker content
WO2012023825A2 (fr) 2010-08-19 2012-02-23 Lg Hausys, Ltd. Composition de pâte pour marbre artificiel et procédé de fabrication de marbre artificiel l'utilisant
CN103068769A (zh) * 2010-08-19 2013-04-24 乐金华奥斯株式会社 人造大理石用糊剂组合物及使用其制造人造大理石的方法
EP2606014A2 (fr) * 2010-08-19 2013-06-26 LG Hausys, Ltd. Composition de pâte pour marbre artificiel et procédé de fabrication de marbre artificiel l'utilisant
EP2606014A4 (fr) * 2010-08-19 2014-01-22 Lg Hausys Ltd Composition de pâte pour marbre artificiel et procédé de fabrication de marbre artificiel l'utilisant
EP3360854A1 (fr) * 2017-02-10 2018-08-15 Holcim Technology Ltd. Composition de ciment blanc ultra-fin

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