# Patent

## Title
Method for continuously coating particulate material

## Abstract

An adhesive-free, dry, free-flowing powder composition suitable for use in surface defect detection, where the powder composition comprises a physical mixture of particles of a colorant and particles of an extender, which mixture includes particles of colorant and particles of extender each having a particle size of less than 100 .mu.m. The powder compositions of the invention provide a simple, effective guide coat which readily highlights surface imperfections, such as scratches, orange peel effect and dry over-spray without the need for solvents. Also, there are disclosed methods of using such a powder composition to detect surface imperfections, an apparatus for applying same, a device for refilling such applying apparatus, and coated surfaces formed thereby.

## Background
This invention relates to a powder composition for use in the detection of defects on surfaces and to its method of use in surface finishing processes. The invention also relates to an applicator means for dispensing and applying such a powder composition.

Many surface finishing processes, particularly repair processes in the automotive refinish industry, involve the application of fillers to imperfections in the surface followed by progressive abrasion with coarser to finer abrasive materials until the desired smooth surface is achieved. A series of protective coatings is applied, e.g., primer, paint coats, lacquers and so forth, and each layer is normally rubbed down prior to application of the next coat in order to ensure a smooth surface.

In order to assist the operator in identifying areas requiring abrasion and highlighting defects during the repair process, it is known to apply a guide coat to the surface being treated. The guide coats generally comprises a dilute paint mixture which is sprayed over the surface to be treated to provide a light paint coating. As the surface is abraded the guide coat is removed from the higher portions of the surface leaving the visible guide coat on the lower areas. Thus, the surface irregularities are clearly visible to the operator, enabling him to abrade and fill the appropriate areas.

The use of a dilute paint mixture as a guide coat suffers from the disadvantages that it is necessary to mask surrounding areas of surface which are not to be treated and the use of large amounts of volatile solvent is undesirable.

The present invention, described hereinafter, provides an alternative system for use as a guide coat.

According to the present invention there is provided an adhesive-free, dry, free-flowing powder composition suitable for use in surface defect detection. The inventive powder composition comprises a physical mixture of particles of a colorant and particles of an extender, which mixture includes particles of colorant and particles of extender each having a particle size of less than 100 .mu.m.

The powder compositions of the invention provide a simple, effective guide coat which readily highlights surface imperfections, such as scratches, orange peel effect and dry over-spray. The compositions do not require the presence of solvents and therefore there is no drying time and the surface may be abraded immediately after application of the guide coat. Furthermore, it has been found that many powder compositions of the invention can substantially reduce the abrading time compared to the use of a guide coat formed by a dilute paint mixture.

FIG. 1 represents a perspective view of an applicator for a powder composition in accordance with the invention.

FIG. 2 represents a cross-section through a reservoir of powder composition.

The powder compositions of the invention are free from adhesive, thereby readily allowing the composition to be distributed readily over a large surface area.

Generally, at least 50%, preferably at least 90% by weight of the particles of the powder composition have a nonzero particle size of less than 100 .mu.m, in order to reveal defects in a surface having dimensions up to 100 .mu.m. Preferably the average particle size of all the particles used is less than 40 .mu.m, more preferably substantially all the particles have a particle size less than 40 .mu.m. It is preferred that the compositions contain some particles less than 10 .mu.m in particle size order to reveal fine scratches. More preferably the average particle size of the powder composition, overall, is about 10 .mu.m. In the present invention, by the terminology "particle size", it is meant the greatest cross-sectional diameter of the particle. These particle sizes can be determined by sieve tray screening.

The colorant is selected to contrast with the surface to which the composition will be applied. In principle, any dry, free-flowing colored particles may be used in the compositions of the invention. However, many organic pigments or dyes are not economical and/or do not spread evenly over the surface. Inorganic colorants are preferred, e.g., carbon black, iron oxide, etc. The most preferred colorant is carbon black, particularly activated carbon black. Mixtures of colorant may be employed.

The extender is generally a light-colored particulate material which dilutes the colorant. Suitable extenders include calcium carbonate, titanium dioxide, talc, magnesium stearate, zinc stearate, calcium stearate and aluminium stearate. The preferred extender in terms of economy and performance is calcium carbonate. Mixtures of extenders may be employed.

The morphology of the particles is not believed to be important providing the particles are free-flowing and will spread evenly. The colorant is generally present in an amount of less than 50% by weight of the composition and is preferably in the range 25 to 40% by weight.

A preferred guide coat composition of this invention comprises about 30-40% by weight carbon black(s) (total, if a combination is used) and about 60-70% by weight calcium carbonate. These components are typically mixed in a rotary blender, for example, until a homogeneous powder is produced. One preferred guide coat composition of the present invention is formulated to involve a physical mixture, by weight, of about 3-15% of a high color strength non-activated carbon black with an activated carbon black in combination with an extender. A particularly preferred composition includes about 66% calcium carbonate (e.g., Snowcal.TM. 30); about 6% of a first type of carbon black (e.g., Raven.TM. 2000D); and about 28% a second type of carbon black except that it is an activated carbon black (e.g., Chemviron Type C). Snowcal.TM. 30 calcium carbonate powder can be commercially obtained from Croxton & Garry Ltd., Dorking, Surrey England, and is composed of 96% calcium carbonate, 2.0% silica, 0.1% ferric oxide, 0.2% alumina, and small residue of copper and lead. As to its physical properties, Snowcal.TM. 30 has a weight medium diameter of 4.6 .mu.m; a specific gravity of 2.7; oil absorption (rub out method) of 15 g/100 g; and the percentage (%) retained on 125 .mu.m sieve is 0.2, % retained on 63 .mu.m sieve is 5.0, and & retained on 45 .mu.m sieve is 12, with the % by weight of particles finer than 2 .mu.m being 30. Raven.TM. 2000D carbon black powder, which is a high color strength non-activated carbon black, commercially available from Columbia Chemicals Co., Atlanta Ga., USA, has a particle size of 18 nm (i.e., the arithmetic mean particle size as measured by electron microscopy); a surface area of about 200 m.sup.2 /g; a DBP oil absorption of 70 cc/100 g; and a powder density of 16 lb./ft.sup.3 (i.e. 2.57.times.10.sup.-2 g/cm.sup.3). Chemviron Type C activated carbon black is commercially available from Chemviron Carbon Limited, Southlink Great Britain, and is a powder activated carbon having iodine number of 900 minutes; a moisture content of 2% maximum; an ash content of 14% maximum; a bulk density of 0.3 to 0.7 g/cm.sup.3 ; and a wet screen analysis through 325 US mesh (approximately 44 .mu.m opening size) of 65 to 85%. About 3-15% of a high color strength non-activated carbon black having an average particle size of less than about 25 .mu.m is particularly desirable for use in the compositions of the present invention because the composition appears to adhere better to painted surfaces, but is relatively easy to remove during both wet and dry sanding operations.

Desirable guide coat compositions would include those achieving as many as possible of the following desired characteristics:

In practice, mixtures of carbon black and chalk of this invention are highly suitable as they fulfill most of these desired properties and are economical as compared with other materials.

The powder composition may be distributed over the surface by any suitable means, e.g., by sprinkling powder onto the surface and spreading with a cloth, pad or sponge. Only small amounts of powder composition are required and it is possible to apply a guide coat to the complete body work of a medium-sized automobile using about 9 grams of powder composition. In practice, the powder composition is generally employed in amounts of from 0.5 to 10 g/m.sup.2 based on the amount of colorant and extender having a particle size of less than 100 .mu.m.

The powder composition will generally be applied to surfaces to which filler has been applied and/or coated with primer, paint lacquer, and so forth, since these are the stages in the refinish industry where guide coats are generally employed. However, the guide coat compositions may be applied directly to non-treated surfaces if required, e.g., wood, metal, such as steel, plastic, fibre glass, and the like.

The powder composition may be stored and dispensed onto the surface from a bag, sachet or container similar to a salt or pepper shaker. Alternatively, the powder composition may be impregnated within the fibres of a fleece, mop, woven or non-woven fabric, or foam which may be wiped over the surface to deposit the powder. In a further embodiment the powder composition may be contained within the reservoir of an applicator and dispensed when the applicator is wiped over the surface. In another embodiment the powder is stored in a reservoir adapted to accommodate the applicator in order to load the applicator with powder prior to use. It is also possible to apply the powder material in a gas stream.

The invention will now be described with reference to the accompanying drawings of FIGS. 1 and 2.

As illustrated in FIG. 1, the applicator means (1) comprises a handle (2) secured to a back-up pad (4) which supports an applicator pad (6). The handle (2) and back-up pad (4) also can be an integral molded body, such as a single integral element of molded rigid foam. The applicator pad (6) may comprise a mop, fleece or foam. A preferred applicator pad is formed of Caligen.TM. 4200 polyester polyurethane foam. Preferably the applicator pads are removable from the back-up pad in order that they may be replaced. Any suitable fixing system may be employed such as those commonly used for attaching abrasive paper to the back-up pads of sanding devices. For example, the foam may be coated with a pressure-sensitive adhesive and adhered to the back-up pad. Alternatively the pad may be laminated to brushed nylon on one surface which cooperates with a hook system provided on the surface of the back-up pad. For instance, the applicator can comprise a layer of molded foam onto which the brushed nylon is laminated to the backside thereof. This brushed nylon, as described above, provides an attachment surface for the hooks of the back-up pad.

In one embodiment of the invention the powder is applied to the applicator pad (6), then applied to a surface, or, the powder is applied directly to the surface to be coated from a separate container.

In a further embodiment of the invention the handle (2) may be hollowed to provide a space for storing a supply of dry guide coat powder. Such a powder storage handle can be associated with a delivery system which will feed powder through the back-up pad (4) and applicator pad to allow application of the powder to a surface. The delivery system may comprise one or more holes through the back-up pad, which may be selectively opened and closed. Alternatively, a feed mechanism such as an Archimedes' screw or a power-assisted mechanism using a spring or compressed gas or propellant may facilitate delivery of the powder from the reservoir to the applicator pad.

In a further embodiment of the invention the applicator pad may be impregnated or loaded with the powder composition and thereafter attached to the back-up pad prior to use.

In another embodiment the applicator pad may be loaded with powder prior to use by use of a refill container device as shown in FIG. 2. The refill container (8) comprises two basic components: an applicator pad support and powder delivery element (10) and a removable hollow cap (15) for storage of powder (12). The element (10) can be an integral member of molded rigid plastic comprising an open end (14); a horizontal, circular apertured surface (20) (such as having radial slot openings or channels (11) therethrough) having a horizontal annular flange (16) at its periphery; an upstanding circumferential rim (18) on its front side; and an upstanding circumferential flange (17) on its back side to permit removable attachment of removable cap element (15) which serves as a storage reservoir for refill powder (12). The outside surfaces of such flange (17) are ribbed to allow for interlocking with protrusion (13) provided on the inside wall of cap member (15), to allow these two members to be removably held together and detachable. The rim (18) is dimensioned to accommodate the applicator pad (6) of the applicator therewithin such that the pad may be supported on the horizontal flange (16). Preferably, the rim (18) has a plurality of circumferentially-spaced lugs or inward projections (tabs) (19) provided on the upper end of the rim (18) to assist in retaining an applicator pad during powder refill or handling. These lugs can be spaced equidistantly around the circumference of the rim end surfaces. The horizontal apertured surface (20) extends across the opening to provide additional support for the applicator pad (6). The element (20), alternatively, can be provided as a separate component attached to the upper surfaces of flange 16, such as where the element (20) is mesh or gauze.

The refill device (8) provides a useful support and replacement powder storage device for the applicator which prevents contamination of the applicator pad (6). The applicator pad (6) is readily loaded with powder by simply inverting or shaking the refill device (10) and applicator assembly, as fitted together. The presence of a uniform array of apertures, such as a plurality of radial slots (11) (e.g., radially eminating from a center of surface (20)) or in mesh or gauze, in element (20), assists in uniform loading of the powder over the surface of the applicator pad (6).

In one mode of the refill device of the invention, a removable, non-apertured separator sheet (not shown) can be interposed between surface (20), and a replacement applicator pad itself (not shown) and similar to pad (6) that is prepackaged within and provided as part of the refill device (8) when sold in commerce, so as to prevent powder flow from the cap reservoir into the replacement pad before usage of the refill device.

The powder composition is readily spread over a surface by application of light pressure to wipe the applicator pad over a surface.

The invention will now be illustrated by the following Examples in which all percentages are by weight unless otherwise indicated.

Test Method

Each powder composition was tested on a primed Rover.TM. 200 bonnet (hood of an automobile) within 24 hours of painting. All work was carried out on a bench with the bonnets in a horizontal plane.

1. Bonnet Preparation

The surfaces were sanded with 3M 255P P180 HOOKIT.TM. 50 mm diameter, 6 hole discs, one per bonnet, using a D/A 5 mm orbital sander with dust extraction.

The swarf was removed with a solvent wipe.

A two-component "2K" primer, described below, was then applied and cured. The primer used was beige in color and comprised:

each commercially available from Herberts, Essex, United Kingdom.

2. Guide Coat Application foam pad.

3. Coating Appearance

The bonnets coated with powder were then compared with that of an aerosol guide coated panel.

4. Sanding

The guide coated surfaces were sanded with 3M 255P P500 HOOKIT.TM. 150 mm diameter, 6 hole discs, one per bonnet, using a D/A 5 mm orbital sander with dust extraction until a visually uniform sanded surface was attained. The areas and the time taken to sand were measured and recorded.

An aerosol guide coated bonnet was used as a control. The aerosol paint used was Spectra.TM. Cellulose Matte Black Spray Paint (Part No. SIMP 17) commercially available from Simoniz International plc, Cornwall, United Kingdom. This product has heretofore been used regularly in United Kingdom body shops as a guide coat. The data from eight experiments on the bonnets were analyzed to establish an overall average sanding time and to give an indication of the deviation of that data from the average. The information can be summarized as follows: Average Sanding Time  5.82 minutes/m.sup.2 per Unit Area Sample Standard Deviation(s) 0.50 ______________________________________

These results were used as a control for the following experiments.

The following materials were tested as guide coats: Columbian Chemicals. Columbian Chemicals. 325 US mesh (45 .mu.m)=96%, commercially available from Chemviron Carbon Limited. through 325 US mesh (45 .mu.m)=65 to 85%, commercially available from Chemviron Carbon Limited. Garry Limited, median diameter 4.6 .mu.m, percentage retained on 45 .mu.m sieve =12% by wt. Garry Limited, median diameter 4.6 .mu.m, percentage retained on 45 .mu.m sieve =12% by wt. Garry Limited, median diameter 2.8 .mu.m, percentage retained on 45 .mu.m sieve =0.02% by wt.

The following 31 different guide coat compositions summarized in Table 1 were prepared by mixing the indicated proportions (in wt. %) of each of carbon black and calcium carbonate. The guide coat compositions summarized in Table 1 were prepared, where, for each composition, the amount by weight % of carbon black contained is indicated in the left-hand column and the amount by weight % of calcium carbonate contained therewith is indicated in the adjacent right-hand column. ______________________________________ Carbon Black   Calcium Carbonate ______________________________________ 5%        R2500    95% Snowcal .TM. 20 7%        R2500    93% Snowcal .TM. 20 11%       R2500    89% Snowcal .TM. 20 10%       R2500    90% Snowcal .TM. 20 10%       R2500    90% Snowcal .TM. 20 15%       R2500    85% Snowcal .TM. 20 20%       R2500    80% Snowcal .TM. 20 20%       R2500    80% Snowcal .TM. 20 30%       R2500    70% Snowcal .TM. 20 35%       R2500    65% Snowcal .TM. 20 5%        R410     95% Snowcal .TM. 20 10%       R410     90% Snowcal .TM. 20 15%       R410     85% Snowcal .TM. 20 20%       R410     80% Snowcal .TM. 20 25%       R410     75% Snowcal .TM. 20 27%       R410     73% Snowcal .TM. 20 35%       R410     65% Snowcal .TM. 20 25%       Type CBX 75% Snowcal .TM. 20 30%       Type CBX 70% Snowcal .TM. 20 30%       Type CBX 70% Snowcal .TM. 20 30%       Type CBX 70% Snowcal .TM. 30 30%       Type CBX 70% Snowcal .TM. 60 32.5%     Type CBX 67.5% Snowcal .TM. 20 35%       Type CBX 65% Snowcal .TM. 20 35%       Type CBX 65% Snowcal .TM. 20 37.5%     Type CBX 62.5% Snowcal .TM. 20 42.5%     Type CBX 57.5% Snowcal .TM. 20 45%       Type CBX 55% Snowcal .TM. 20 30%       Type C   70% Snowcal .TM. 20 30%       Type C   70% Snowcal .TM. 30 30%       Type C   70% Snowcal .TM. 60 ______________________________________

The guide coat compositions described above in Table 1 were evaluated by the test method described above. All of the above compositions proved to be acceptable as guide coats having a sanding time per unit area in the range 3.5 to 5 minutes, which is less than the average time required using conventional aerosol paint as a guide coat.

Compositions having higher carbon black content were darker but provided no obvious advantage in terms of sanding time. Activated carbon black was more effective than non-activated carbon black. Composition comprising 25 to 40% by weight carbon black are preferred in terms of acceptable performance and economy.

The sanding performance of five dry powder guide coat systems was compared with a black aerosol guide coat using the above test method. The powders for each test powder sample of this example comprised 30% by weight carbon black and 70% by weight calcium carbonate. The results are indicated in Table 2. ______________________________________ Sanding Time Per Unit Area Black Guide Coats (minutes/m.sup.2) ______________________________________ Type CBX/Snowcal .TM. 20 4.34 Type CBX/Snowcal .TM. 60 4.36 Type C/Snowcal .TM. 20 4.45 Type C/Snowcal .TM. 30 3.63 Type C/Snowcal .TM. 60 3.56 Simoniz, Aerosol (control) 5.82 ______________________________________

This experiment investigated whether powder paints, in the form of the water dispersible products currently available in many retail stores, would be suitable as guide coats. The black powder paints used generally comprise a mix of pigment (carbon black), adhesive (starch) and filler (calcium carbonate); their proportions vary depending upon their end use and the manufacturer. Black powder paints from the Early Learning Centre (ELC), Calder Colours and Partners were used. The test method described above was again used. The results are summarized in Table 3. ______________________________________ Sanding Time Per Black Guide Unit Area   Application Coats    (minutes/m.sup.2) Comments   Sanding Comments ______________________________________ ELC, Powder 6.06        too dark,  swarf stains, streaky coating marks left on paint Calder,  6.16        too dark,  swarf stains, Playgroup            streaky coating marks left on Powder                          paint Calder, Art 5.79        too dark,  swarf stains, Powder               streaky coating marks left on paint Partners, 6.29        too dark,  swarf stains, Powder               streaky coating marks left on paint ______________________________________

The appearance of the bonnets coated with the powder paints were unacceptable when compared with the aerosol spray paint guide coated bonnet. The coatings were too dark and very streaky.

The swarf created while sanding the bonnets coated with the powder paints stained the newly sanded surfaces. All the bonnets coated with the powder paints took longer to sand than the aerosol spray paint guide coated bonnet.

The following powders were tested as guide coats:

In Table 4, the results observed upon subjecting each of the above powder formulations to the test method are summarized. The mixing proportions, if any, as described above for the various powder formulations studied for this example, are omitted from Table 4 merely for the sake of brevity. ______________________________________ Sanding Time per Unit Area Guide Coats   (minutes/m.sup.2) Comments ______________________________________ Type C        4.80         too dark, streaky Snowcal .TM. 20 .about.3.8   too light, difficult to evaluate Talc          .about.3.62  too light, difficult to evaluate Type MT/Snowcal .TM. 20 3.76 Type C/Talc   3.80         difficult to evaluate Type C/Stearic Acid 5.9          forms spheres on surface Type C/TiO.sub.2 4.0 Type C/Zn Stearate 4.5 Type C/Ca Stearate 4.2 Type C/Al Stearate 5.9 ______________________________________

All the powder guide coated panels sanded faster than the aerosol spray paint guide coated panel.

It was difficult to decide whether the bonnet coated with Snowcal.TM. 20 and the bonnet coated with talc were completely sanded as their coatings were almost invisible. Defects were undetectable on the bonnets coated with Snowcal.TM. 20 and talc, the powders were unable to highlight them.

Whilst talc, TiO.sub.2 and stearates may be used as extenders they do not appear to offer advantages over calcium carbonate.

Tests were conducted using compositions consisting of 30% colorant and 70% Snowcal.TM. 30 (by wt.), with the colorant changed as indicated in the following descriptions of the compositions studied:

The colorants each used with 70% Snowcal.TM. 30 were: commercially available from BASF. The powders were subjected to the above test method and the results are summarized in Table 5. ______________________________________ Sanding Time per Unit Area Guide Coat     (minutes/m.sup.2) Comments ______________________________________ Sico Red/Snowcal .TM. 30 6.8           too dark Heliogen       7.0           too dark, swarf Blue/Snowcal .TM. 30         stains Green Art      .about.3.8    too light, Powder/Snowcal .TM. 30       difficult to evaluate Red Iron       4.8           dark oxide/Snowcal .TM. 30 Milori         5.9           too dark, swarf Blue/Snowcal .TM. 30         stains Simoniz, Aerosol. 5.82 (control) ______________________________________

Whilst all the guide compositions were useful to some degree, the colorants tested did not appear to be optimal as compared to carbon black. Iron oxide was the best alternative to carbon black.

## Claims

1. A method of forming a guide coat on a surface to detect defects thereon which comprises distributing over the surface an adhesive-free, dry, free-flowing powder composition consisting essentially of particles of a colorant selected from the group consisting of carbon black and iron oxide and particles of an extender selected from the group consisting of calcium carbonate, titanium dioxide, talc, magnesium stearate, zinc stearate, calcium stearate and aluminum stearate, wherein said particles of colorant and said particles of extender each include fine particles having a particle size of less than 100 .mu.m.

2. The method of claim 1 in which at least 50% by weight of all said particles of colorant and extender have a particle size of less than 100 .mu.m.

3. The method of claim 1 in which an average particle size of all said particles is less than 40 .mu.m.

4. The method of claim 3 having an average particle size of approximately 10 .mu.m.

5. The method of claim 1 in which all fine particles have a particle size less than 10 .mu.m.

6. The method of claim 1 in which the colorant comprises activated carbon black.

7. The method of claim 1 in which said extender is calcium carbonate.

8. The method of claim 1 in which said colorant is present in an amount of less than 50% by weight of said composition.

9. The method of claim 8 in which said colorant comprises a mixture of two types of carbon black.

10. The method of claim 9 in which one of said types of carbon black is an activated carbon black.

11. The method of claim 1 wherein all of the particles consist essentially of from about 25% to about 40% by weight carbon black and from about 60% to about 75% by weight of calcium carbonate.

12. The method of claim 11 wherein all of the particles consist essentially of about 28% activated carbon black, about 6% non-activated carbon black, and about 66% by weight of calcium carbonate.

13. A method of sanding a surface which comprises applying to said surface a guide coat comprising an adhesive-free dry, free-flowing powder composition consisting essentially of particles of a colorant selected from the group consisting of carbon black and iron xide and particles of an extender selected from the group consisting of calcium carbonate, titanium dioxide, talc, magnesium stearate, zinc stearate, calcium stearate and aluminum stearate, wherein said particles of colorant and said particles of extender each include fine particles having a particle size of less than 100 .mu.m and thereafter sanding the guide coated surface.