WO2016185023A1

WO2016185023A1 - A method and punch for pressing sticky material samples for x-ray analysis

Info

Publication number: WO2016185023A1
Application number: PCT/EP2016/061438
Authority: WO
Inventors: Michal KRSEK; Vladimir MELEG
Original assignee: FLSmidth AS
Current assignee: FLSmidth AS
Priority date: 2015-05-21
Filing date: 2016-05-20
Publication date: 2016-11-24
Anticipated expiration: 2017-11-21

Abstract

A punch (1100) for use in a sample preparation apparatus configured to prepare a sticky material sample suitable for X-ray analysis comprising an upper surface part (1103) and a lower surface part (1104) having an outer flat ring (1101) and a pressing surface part (1102); wherein at least a portion of the punch is coated with a diamond-like carbon coating configured to reduce the amount of sticky material residue on the punch after preparation of the sticky material sample. Also disclosed are methods for preparing a non-contaminated material sample suitable for X-ray analysis.

Description

A METHOD AND PUNCH FOR PRESSING STICKY MATERIAL SAMPLES FOR

X-RAY ANALYSIS

FIELD OF THE INVENTION

This invention relates to sample preparation equipment and methods, and most particularly to a punch for systems for preparing X-ray samples (XRF or XRD analysis technique) in minerals processing industries. BACKGROUND OF THE INVENTION

XRD and XRF are rapid analytical technique primarily used to determine concentrations of sample elements or for phase identification of a crystalline material. The technique generally involves the steps of providing sample material, finely grinding the sample material, homogenizing the finely-ground sample material, and determining the average bulk composition of the homogenized sample.

Several X-ray sample preparation systems are already on the market for example:

Polysius (ThyssenKrupp) offers the Polab® APM Automatic Sample Preparation Module; Herzog offers the HP-PD6 automated press for use with dry powder having a grain of ΘΟμηη; and Essa Australia (now a subsidiary of FLSmidth, the Applicant) offers the semi- automated Essa® XRD Press. However, the existing X-ray sample preparation systems, such as those mentioned herein, fail to address objects of the present invention in that they are unable to handle a wide range of materials due to cross contamination of samples. In particular, such machines are susceptible to cross contamination of samples when handling sticky materials such as lime or hydrated lime because residue is left on the punch or die press. This means that more cleaning and human intervention is necessary and that more consumables are required. The aforementioned reduces throughput and increases cost.

It will be clearly understood that any reference herein to background material or information, does not constitute an admission that any material, information, forms part of the common general knowledge in the art, or is otherwise admissible prior art. OBJECT OF THE INVENTION

It is an object of the invention to overcome or at least alleviate one or more of the above problems and/or provide the consumer with a useful or commercial choice.

SUMMARY OF THE INVENTION A punch for use in a sample preparation apparatus configured to prepare a sticky material sample suitable for X-ray analysis is provided. The punch may comprise an upper surface part and a lower surface part having an outer flat ring and a pressing surface part; wherein at least a portion of the punch is coated with a diamond-like carbon coating configured to reduce the amount of sticky material residue on the punch after preparation of the sticky material sample.

In some embodiments, at least a portion of the upper surface part or lower surface part is coated with a diamond-like carbon coating configured to reduce the amount of sticky material residue on the punch after preparation of the sticky material sample.

In some embodiments, the lower surface part is completely coated with a diamond-like carbon coating configured to reduce the amount of sticky material residue on the punch after preparation of the sticky material sample.

In some embodiments, the diamond-like carbon coating is comprised of an adhesive layer and a top layer. In some embodiments, the adhesive layer may be less than or equal to .08 μηη thick. In some embodiments, the top layer may be less than or equal to 1 .5 μηη thick. In some embodiments, the adhesive layer is comprised of tungsten, carbon, hydrogen and chromium. In some embodiments, the top layer is comprised of carbon and hydrogen.

Also provided is a method of preparing a non-contaminated material sample suitable for X-ray analysis. The method may comprise: introducing a first sticky material sample into a sample preparation apparatus; pressing the sticky material sample with the punch as described herein; removing the pressed sticky material sample from the sample preparation apparatus; introducing a second material sample into the sample apparatus; pressing the second material sample with the punch as described herein; removing the pressed second material sample from the preparation apparatus. In some embodiments the method may be automated. Also provided is a method of preparing a non-contaminated material sample suitable for X-ray analysis. The method may comprise: coating at least a portion of a punch with a diamond-like carbon coating, the coating being configured to reduce the amount of sticky material residue on the punch after preparation of the sticky material sample; providing the punch into a sample preparation apparatus; pressing a sticky material sample:

removing the sticky material sample from the sample preparation apparatus.

Other details, objects, and advantages of the invention will become apparent as the following description of certain present exemplary embodiments thereof and certain present exemplary methods of practicing the same proceeds. BRIEF DESCRIPTION OF THE DRAWINGS

Embodiments of the invention, by way of example only, will be described with reference to the accompanying drawings in which:

Figure 1 shows an exemplary sample preparation apparatus, more particularly a first version of FLSmidth's Centaurus™ machine. Figure 2 shows an exemplary sample preparation apparatus, more particularly a second version of FLSmidth's Centaurus™ machine.

Figure 3 shows a portion of an exemplary preparation apparatus particularly a first version of FLSmidth's Centaurus™ machine.

Figure 4 shows a punch installed above a press which is configured to form a pressed material sample.

Figure 5 shows a pressed material sample and the punch and press.

Figure 6 shows an exemplary embodiment of a punch for use in a sample preparation apparatus configured to prepare a sticky material sample suitable for XRD.

Figure 7 shows a lightly pressed prepared XRD material sample formed within an annular sample holder according to some embodiments.

Figure 8 is a schematic representation of an XRD sample preparation apparatus including a punch according to some embodiments. Figure 9 shows an exemplary embodiment of a punch coated with a diamond-like carbon coating.

DETAILED DESCRIPTION OF THE INVENTION

Referring to Figures 1 through 3, exemplary sample preparation apparatuses 1 are shown. Figure 1 shows a first version of FLSmidth's Centaurus™ machine with the cover panel closed. In some embodiments, the sample preparation apparatus 1 may have a grinding aid pellet dispenser 2 where in some embodiments grinding pellets are dispensed into the sample preparation apparatus 1 automatically to assist with grinding of material. The sample preparation apparatus may also have material sample entry points 3, 4 where material to be prepared for XRD is introduced into the sample preparation apparatus. In an exemplary embodiment, there may be a first sample entry point 3 where samples enter the machine via an operator or a robot. There may also be a second sample entry point 4 where samples arrive via a transport belt or from an optional input magazine (not shown). The sample apparatus 1 may also have a first sample output point 6 where an operator or robot may collect prepared material samples from the front of the apparatus. In some embodiments, the sample preparation apparatus 1 may have an optional output or input point 5 (output point for grinding only samples and input point for pressing only samples).

Figure 2 shows a second version of FLSmidth's Centaurus™ machine. The exemplary sample preparation apparatus 1 , shown in Figure 2 has e.g. a first sample entry point 3 where samples enter the machine via an operator or a robot, a first sample output point 6 where an operator or robot may collect prepared material samples from the front of the apparatus and a second material outpoint point where, in a linear or conventional system, a pressed material sample can be collected by an external conveyor belt (not shown) that is able to transport the tablet directly to a XRD analyser.

Figure 3 shows the first version of FLSmidth's Centaurus™ machine with the cover panel open and detail of pressing tool. As shown, a sample preparation apparatus 1 may have a punch 1 100, a press 1200, a platen 1202 and springs 1208.

The punch 1 100 of the current invention (described below) may be used in any sample preparation apparatus that produces material samples for X-ray analysis, such as the sample preparation apparatuses shown in Figures 1 -3. FIG. 4 shows a punch 1 100 according to some non-limiting embodiments. The punch 1 100 may be installed above a lower press 1200. The lower press 1200 may have a platen 1202 and one or more springs 1208 may be provided to an XRF/XRD sample preparation apparatus 1 . The press 1200 may be a lower cartridge press which moves the platen 1202 upwards, towards the punch 1 100 which may be stationary with respect to other components of the XRF/XRD sample preparation apparatus 1. At least a portion of the punch 1 100 is coated with a diamond-like carbon coating. The diamond-like carbon coating reduces the amount of sticky material residue on the punch 1 100 after preparation of a sticky material sample. In some embodiments, the diamond-like carbon coating is comprised of an adhesive layer and a top layer. In one embodiment, the adhesive layer is equal to or less than .08 pm. In one embodiment, the top layer is equal to or less than 1 .5 pm. In one embodiment the adhesive layer is comprised of Tungsten, Carbon, Hydrogen and Chromium. In one embodiment, the top layer is comprised of Carbon and Hydrogen. FIG. 5 shows the operation of pressing an XRF/XRD material sample utilizing the punch 1 100 of the sample preparation apparatus described herein. The mounted punch 1 100, wherein at least a portion of the punch 1 100 is coated with the diamond-like carbon coating, operated by pneumatic cylinder moves downward to a defined position; during pressing, the punch 1 100 is fixed in position. One or more retaining claws 1204 may engage a retaining groove 403 of the sample holder assembly 600 to secure it to a movable platform/cartridge 1206 which is guided by a track 1220. The pressing forces that are utilized to prepare a completed sample briquette 900' may vary and depends if the sample has to be analyzed by XRF or XRD technique.

FIG. 6 shows an exemplary embodiment of the punch 1 100. In some embodiments, as shown, the punch 1 100 may be composed of an upper surface part 1 103, a lower surface part 1 104 having an outer flat ring 1 101 and a pressing textured surface part 1 102. In cases where a flat punch is used, the punch 1 100 may be comprised of a single piece part. In some embodiments of the punch 1 100, at least a portion of the upper surface part 1 103 or lower surface part is coated with a diamond-like carbon coating configured to reduce the amount of sticky material residue on the punch 1 100 after preparation of the sticky material sample. In other embodiments, the lower surface part 1 104 is completely coated with a diamond-like carbon coating configured to reduce the amount of sticky material residue on the punch 1 100 after preparation of the sticky material sample. FIG. 7 shows a lightly pressed, prepared XRD material sample pellet 900' formed within a sample holder assembly 600 according to some embodiments. The XRD material sample or briquette 900' has an upper exposed measuring surface which is configured to be used in an XRD measuring test. FIG. 8 is a schematic representation of an XRD sample preparation apparatus according to some embodiments. A dished sample holder bottom 500 fits within the annular sample holder 400, and finely-ground sample material 900 is dosed within the annular sample holder 400 such that it rests on the concave dished surface 501 of the dished sample holder bottom 500. A punch 1 100 wherein at least a portion of the punch 1 100 is coated with the diamond-like carbon coating, comes into contact with the sample material 900, and applies a force to the sample material 900. The concave dished surface 501 of the dished sample holder bottom 500 evenly distributes the sample material 900 granules around the annular sample holder (i.e., radially outwardly) as pressing forces gradually increase. Since the dished sample holder bottom 500 is movable with respect to the punch 1 100 and annular sample holder 400, along the same axis, excess pressure exerted by the punch 1 100 simply moves the granules within the sample holder assembly 600 around (e.g., outward within the annular sample holder 400.

FIG. 9 shows the punch 1 100 wherein the entire punch 1 100 is coated with a diamond- like carbon coating. The diamond-like carbon coating on the punch 1 100 allows a sample preparation apparatus 1 to handle a wide range of materials without cross contamination between material samples. For example, a sticky material, such as hydrated lime, could be pressed by the punch 1 100. Because of the diamond-like carbon coating, the residue from the hydrated lime on the punch 1 100 is reduced and/or eliminated. Because there is little or no residue no cleaning is necessary before another material sample is introduced into the sample preparation apparatus. As a result, less consumables are required, and less human intervention is necessary which increases throughput and decreases material sample preparation costs.

It is to be understood that the form of this invention as shown is merely a preferred embodiment. Various changes may be made in the function and arrangement of parts; equivalent means may be substituted for those illustrated and described; and certain features may be used independently from others without departing from the spirit and scope of the invention as defined in the following claims. List of Components:

1 sample preparation apparatus

2 grinding aid pellet dispenser

3 first sample entry point

4 second sample entry point

5 optional output or input point

6 first tablet output point

400 annular sample holder

500 dished sample holder bottom

501 dished surface (i.e., concave)

403 retaining groove

600 sample holder assembly

900 sample material

900' pressed sample pellet for X-ray analysis

1 100 punch

1 101 boss (optional)

1 102 flat/textured/sanded surface

1 103 upper surface

1 104 lower surface

1200 press

1202 platen

1204 retaining claw

1206 cartridge/platform

1208 springs

Claims

1 . A punch (1 100) for use in a sample preparation apparatus configured to prepare a sticky material sample suitable for X-ray analysis comprising:

an upper surface part (1 103) and a lower surface part (1 104) having an outer flat ring (1 101 ) and a pressing surface part (1 102);

wherein at least a portion of the punch (1 100) is coated with a diamond-like carbon coating configured to reduce the amount of sticky material residue on the punch (1 100) after preparation of the sticky material sample.

2. The punch of claim 1 , wherein at least a portion of the upper surface part (1 103) or lower surface part is coated with a diamond-like carbon coating configured to reduce the amount of sticky material residue on the punch (1 100) after preparation of the sticky material sample.

3. The punch of claim 1 , wherein the lower surface part is completely coated with a diamond-like carbon coating configured to reduce the amount of sticky material residue on the punch (1 100) after preparation of the sticky material sample.

4. The punch of claim 1 , wherein the diamond-like carbon coating is comprised of an adhesive layer and a top layer.

5. The punch of claim 4, wherein the adhesive layer is less than .08 μηη thick.

6. The punch of claim 4, wherein the top layer is less than 1 .5 μηη thick.

7. The punch of claim 4, wherein the adhesive layer is comprised of tungsten, carbon, hydrogen and chromium.

8. The punch of claim 4, wherein the top layer is comprised of carbon and hydrogen.

9. A method of preparing a non-contaminated material sample (900') suitable for X- ray analysis comprising:

introducing a first sticky material sample (900) into a sample preparation apparatus;

pressing the sticky material sample (900) with the punch (1 100) of any one of claims 1 -8;

removing the pressed sticky material sample (900') from the sample preparation apparatus;

introducing a second material sample (900) into the sample apparatus;

pressing the second material sample (900) with the punch (1 100) of any one of claims 1 -8;

removing the pressed second material sample (900') from the preparation apparatus.

10. The method of claim 9, wherein all steps are automated.

1 1 . A method of preparing a non-contaminated material sample (900') suitable for X- ray analysis comprising:

coating at least a portion of a punch (1 100) with a diamond-like carbon coating, the coating being configured to reduce the amount of sticky material residue on the punch (1 100) after preparation of the sticky material sample;

providing the punch into a sample preparation apparatus;

pressing a sticky material sample (900);

removing the sticky material sample (900') from the sample preparation apparatus.