ROCK DRILL INSERT

Abstract

A rock drill insert made of cemented carbide includes hard constituents of tungsten carbide (WC) in a binder phase of Ni—Cr, or Ni—Co—Cr, and a balance of WC and unavoidable impurities. The cemented carbide has a 3.5-18 wt % binder phase. The binder phase has >0 wt % Ni. The mass ratio Cr/(Ni+Co) is 0.02-0.19. A difference between the hardness at 0.3 mm depth at some point of the surface of the rock drill insert and the minimum hardness of the bulk of the rock drill insert is at least 30 HV3.

Claims

1. A rock drill insert made of cemented carbide that comprises hard constituents of tungsten carbide (WC) in a binder phase of Ni—Cr, or Ni—Co—Cr, and a balance of WC and unavoidable impurities, wherein the cemented carbide comprises 3.5-18 wt % binder phase, the binder phase having >0 wt % Ni, wherein a mass ratio of Cr/(Ni+Co) is 0.02-0.19, and wherein a difference between the hardness at 0.3 mm depth at a point of a surface of the rock drill insert and a minimum hardness of a bulk of the rock drill insert is at least 30 HV3.

2. The rock drill insert according to claim 1, wherein the difference between the hardness at 0.3 mm depth below the surface at the point of the rock drill insert and the hardness at 1 mm below the surface is at least 20 HV3.

3. The rock drill insert according to claim 1, wherein the difference between the average hardness at 0.3 mm below the surface of the rock drill insert and an average hardness in the bulk of the rock drill insert is at least 20 HV3.

4. The rock drill insert according to claim 1, wherein the difference between an average hardness at 0.3 mm below the surface of the rock drill insert and an average hardness at 1 mm below the surface is at least 15 HV3.

5. The rock drill insert according to claim 1, wherein the difference between the hardness at 0.3 mm depth below the surface at any point of the rock drill insert and the minimum hardness of the bulk of the rock drill insert is at least 20 HV3.

6. The rock drill insert according to claim 1, wherein the difference between the hardness 0.3 mm below the surface at any point of the rock drill insert and the hardness at 1 mm below the surface of the rock drill insert is at least 15 HV3.

7. The rock drill insert according to claim 1, wherein a WC grain size mean value of the cemented carbide is above 1 μm but less than 18 μm.

8. The rock drill insert according to claim 1, wherein the cemented carbide includes 4-12 wt % binder phase.

9. The rock drill insert according to claim 1, wherein the binder phase of Ni—Co—Cr has >25 wt % Ni.

10. The rock drill insert according to claim 1, wherein the binder phase of Ni—Co—Cr has >50 wt % Ni.

11. The rock drill insert according to claim 1, wherein the binder phase is a binder phase of Ni—Cr.

12. The rock drill insert according to claim 1, wherein the mass ratio of Cr/(Ni+Co) in the cemented carbide is 0.04-0.19.

13. The rock drill insert according to claim 1, wherein the mass ratio of Cr/(Ni+Co) in the cemented carbide is 0.085-0.15.

14. The rock drill insert according to claim 1, wherein said cemented carbide has a hardness of not higher than 1700 HV3.

15. A rock drill bit body comprising one or more mounted rock drill inserts according to claim 1.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0040] In FIG. 2-9, the ΔHV3 represents the difference between the hardness (HV3) at a certain position and the average hardness as measured in the bulk.

[0041] FIG. 1 is a schematic representation of the geometry of a rock drill insert used in testing.

[0042] FIG. 2 shows a HV3 map with ΔHV3 isolines of an untreated (=as sintered) rock drill insert where the cemented carbide contains 5.6 wt % nickel but no chromium (Sample 1).

[0043] FIG. 3 shows a HV3 map with ΔHV3 isolines of a high-energy oscillation collision treated (27 min) rock drill insert where the cemented carbide contains 5.6 wt % nickel but no chromium (Sample 1).

[0044] FIG. 4 shows an enlarged HV3 map with ΔHV3 isolines of a part of a high-energy oscillation collision treated (27 min) rock drill insert where the cemented carbide contains 5.6 wt % nickel but no chromium (Sample 1).

[0045] FIG. 5 shows a HV3 map with ΔHV3 isolines of a high-energy oscillation collision treated (60 min) rock drill insert where the cemented carbide contains 5.6 wt % nickel but no chromium (Sample 1).

[0046] FIG. 6 shows a HV3 map with ΔHV3 isolines of an untreated rock drill insert where the cemented carbide contains 4.9 wt % nickel and 0.5 wt % chromium (Sample 2).

[0047] FIG. 7 shows a HV3 map with ΔHV3 isolines of a high-energy oscillation collision treated (27 min) rock drill insert where the cemented carbide contains 4.9 wt % nickel and 0.5 wt % chromium (Sample 2).

[0048] FIG. 8 shows an enlarged HV3 map with ΔHV3 isolines of a part of a high-energy oscillation collision treated (27 min) rock drill insert where the cemented carbide contains 4.9 wt % nickel and 0.5 wt % chromium (Sample 2).

[0049] FIG. 9 shows a HV3 map with ΔHV3 isolines of a high-energy oscillation collision treated (60 min) rock drill insert where the cemented carbide contains 4.9 wt % nickel and 0.5 wt % chromium (Sample 2).

[0050] FIG. 10 shows a schematic drawing of a pendulum hammer test set-up (see Example 4).

EXAMPLES

Example 1, Comparative, Ni-Based Cemented Carbide without Cr

[0051] As a first material used a cemented carbide material with 5.6 wt % Ni and balance WC was made according to established cemented carbide processes. Powders of WC, Ni and W were milled in a ball mill together with cemented carbide milling bodies. The WC powder grain size measured as FSSS was before milling between 5 and 8 μm. The milling was carried out in wet conditions, using 92% ethanol, with an addition of 2 wt % polyethylene glycol (PEG 8000) as organic binder. After milling, the slurry was spray-dried in N.sub.2-atmosphere. Green bodies of a desired shape were produced by uniaxial pressing and sintered by using Sinter-HIP in 55 bar Argon-pressure at 1500° C. for 1 hour.

[0052] This material is denoted Sample 1.

Example 2, Invention, Ni-Based Cemented Carbide with Cr

[0053] As a second material used a cemented carbide material with 4.9 wt % Ni, 0.5 wt % Cr and balance WC was made according to established cemented carbide processes. Powders of WC, Ni, Cr.sub.3C.sub.2 and W were milled in a ball mill. The WC powder grain size measured as FSSS was before milling between 5 and 8 μm. The milling was carried out in wet conditions, using ethanol, with an addition of 2 wt % polyethylene glycol (PEG 8000) as organic binder (pressing agent) and cemented carbide milling bodies. After milling, the slurry was spray-dried in N.sub.2-atmosphere. Green bodies of a desired shape were produced by uniaxial pressing and sintered by using Sinter-HIP in 55 bar Ar-pressure at 1500° C. for 1 hour.

[0054] This material is denoted Sample 2.

[0055] Details on the sintered material are given in Table 1.

TABLE-US-00001 TABLE 1 Details on materials produced according to examples 1-2. Reference Cr-grade Sample 1 Sample 2 Ni (wt %) 5.6 4.9 Cr (wt %) — 0.5 C (wt %) 5.7 5.7 W (wt %) 88.7 88.9 Vol % binder (fcc)** 10.8 10.8 Density (g/cm3) 15.10 15.00 HV20* 1282 1392 *Vickers indentations using 20 kg load **Calculated with Thermo-Calc software and TCFE7 database

WC Grain Sizes of Sintered Samples of Examples 1-2

[0056] The mean WC grain sizes of the sintered materials (Sample 1 and Sample 2) according to Examples 1-2 were determined from SEM micrographs showing representative cross sections of the materials. The final step of the sample preparation was carried out by polishing with 1 μm diamond paste on a soft cloth, followed by etching with Murakami solution. SEM micrographs were obtained using the backscatter electron detector (BSE), at 15 kV acceleration voltage and a working distance of 10 mm. The magnifications used were 3000× for the materials Sample 1 and 4000×Sample 2.

[0057] The mean WC grain size was evaluated using the Jeffries method described below, from at least two different micrographs for each material. An average value was then calculated from the mean grain size values obtained from the individual micrographs (for each material respectively). The procedure for the mean grain size evaluation using a modified Jeffries method was the following:

[0058] A rectangular frame of suitable size was selected within the SEM micrograph so as to contain a minimum of 300 WC grains. The grains inside the frame and those intersected by the frame are manually counted, and the mean grain size is obtained from equations (1-3):

[00001]$\begin{array}{cc}M=\frac{L_{\mathrm{scale}\mathrm{mm}}\times {10}^{-3}}{L_{\mathrm{scale}\mathrm{micro}}\times {10}^{-6}}& \left(1\right)\\ \mathrm{vol}\%\mathrm{WC}=100\times \left(-1.308823529\times \frac{\left(\frac{\mathrm{wt}\%\mathrm{Co}}{100}-1\right)}{\left(\frac{\mathrm{wt}\%\mathrm{Co}}{100}+1.308823529\right)}\right)& \left(2\right)\\ d=\frac{1500}{M}\times \sqrt{\frac{L_1\times L_2\times \mathrm{vol}\%\mathrm{WC}}{\left(n_1+\frac{n_2}{2}\right)\times 100}}& \left(3\right)\end{array}$

[0059] Where:

[0060] d=mean WC grain size (μm)

[0061] L.sub.1, L.sub.2=length of sides of the frame (mm)

[0062] M=magnification

[0063] L.sub.scale mm=measured length of scale bar on micrograph in mm

[0064] L.sub.scale micro=actual length of scale bar with respect to magnification (μm)

[0065] n.sub.1=no. grains fully within the frame

[0066] n.sub.2=no. grains intersected by frame boundary

[0067] wt % Co=known cobalt content in weight %.

[0068] Equation (2) is used to estimate the WC fraction based on the known Co content in the material. Equation (3) then yields the mean WC grain size from the ratio of the total WC area in the frame to the number of grains contained in it. Equation (3) also contains a correction factor compensating for the fact that in a random 2 D section, not all grains will be sectioned through their maximum diameter.

[0069] Table 2 shows the mean WC grain size values obtained for the materials according to Examples 1-2 (Sample 1 and Sample 2) with the above described procedure.

TABLE-US-00002 TABLE 2 Mean WC grain size (μm) Sample material (modified Jeffries method) Sample 1 2.6 (According to Example 1) Sample 2 1.8 (According to Example 2)

Example 3, Drill Bit Inserts and their Treatment

[0070] Drill bit inserts were made of a material according to the description in Examples 1 and 2 respectively. The inserts had a size of 10.0 mm in outer diameter (OD) and 16.6 mm in height with a weight of approximately 16.6 g each and having a spherical dome (“cutting edge”). The inserts were ground on the negative part but leaving the dome and bottom part in an as-sintered condition. Some of the inserts were treated using a method that can best be described as a high energy oscillating collision method, hereafter referred to as the E-method. The equipment used is a commercially available paint shaker of trade mark Corob™ Simple Shake 90 with a maximum load of 40 kg and a maximum shaking frequency of 65 Hz. The E-method is based on a rapid oscillating movement of a closed container filled with inserts or a combination of inserts and tumbling media, wherein the container is repeatedly subjected to acceleration peaks typically up to 8.8 g at the shaking frequency of 45 Hz, where g=9.81 m/s.sup.2. The oscillating movement occurs primarily along the z-axis, i.e. the vertical axis, with an amplitude of several cm, and simultaneous movement of lesser intensity along the y-axis in the horizontal plane. The inserts are set in motion by means of impacts with the walls of the moving container and subsequent impacts with other inserts and tumbling media. The high frequency of the velocity vector reversal (i.e. frequent abrupt changes in the direction of motion) results in a large number of high-energy insert collisions per unit of time. This characteristic property of the E-method makes it possible to obtain the desired effect in the treated inserts already after very short treatment times.

[0071] The program used for the E-method insert treatments corresponded to a shaking frequency of 45 Hz. 5-20 rock drill inserts were placed in hard and thermostable plastic container with double lids and dimensions of 133 mm in height and 122 mm in diameter, together with 4.5 kg media (hard metal pellets with a spherical top and bottom and a negative part in between; total height=6.95 mm, the height of the negative part being 3.22 mm and the diameter of the negative part=6.67 mm, of Sandvik grade H10F and with a weight of each pellet about 3 g) and 1-2 dl cold water for cooling. The filling height in the containers was about ½ and should not exceed ¾. One to four containers were clamped automatically and the shaking was then started. The frequency used was 45 Hz and the shaking time was 27 min for some inserts and 60 min for some inserts. To prevent the containers from excessive heating and melting, cooling of the containers had to be performed after 9 min during the treatment.

[0072] The E-treatment has been shown to significantly increase the resistance towards earlier failure due to high impact forces but also, since the effect of the treatment is present all around the drill bit insert, it will also prevent other types of insert failures during handling. The method also gives a significant increase of the hardness (HV3) all over of the surface and a few mm inwards of the insert compared to the bulk hardness (=initial sintered hardness).

Example 4, Drill Bit Inserts and their Treatment

[0073] Further drill bit inserts were made according to the description in Examples 1 and 2 respectively. The inserts had a size of 7.3 mm in outer diameter (OD) and 9.8 mm in height with a weight of approximately 4.8 g each and having a spherical dome (“cutting edge”). The inserts were ground on the negative part but leaving the dome and bottom part in an as-sintered condition. Some of the inserts were treated using The “E-method” as described in Example 3, except for that the shaking time was 9 minutes.

Example 5, Hardness Measurements

[0074] The hardening induced by the high energy surface treatment can be characterized by means of performing Vickers hardness mapping. The inserts are sectioned along the longitudinal axis and polished using standard procedures. Vickers indentations at 3 kg load are then systematically distributed over the polished section. For a more detailed description of the applied method, see below:

[0075] The hardness measurements were performed using a programmable hardness tester, KB30S by KB Prüftechnik GmbH calibrated against HV3 test blocks issued by Euro Products Calibration Laboratory, UK. Hardness is measured according to ISO EN6507. HV3 means 3 kg load, HV5 means 5 kg load, etc.

[0076] The HV3 measurements were done in the following way: [0077] Scanning the edge of the sample. [0078] Programming the hardness tester to make indentations at defined distances to the edge. [0079] Programming the distances between the indentations to 0.3 mm or more. [0080] Indentation with 3 kg load at all programmed coordinates. [0081] Computer moves stage to each coordinate with indentation and runs auto adjust light, auto focus and then auto measure the size of each indentation. [0082] User inspects all photos of the indentations for focus and other matters that disturb the result.

[0083] Actual distance could be found out in the figures by measuring the distance between the “⋄” symbols that mark the actual location of the HV3 indentation in the figure and then correlating with the mm scale given in the X and Y axis.

[0084] The reason for using hardness values measured 0.3 mm below the surface is that with the Vickers indentation method used herein it is difficult to measure the hardness at the very surface.

[0085] FIG. 2-9 show hardness maps (HV3 maps) of the results of the indentations made for drill bit inserts of Sample 1 and Sample 2 (according to Example 3).

[0086] Table 3 shows average hardness values per contour (all HV values measured at a given distance below surface) for Sample 1 and Sample 2 treated according to Example 3.

TABLE-US-00003 TABLE 3 HV3 average 4.8 mm HV3 (0.3 mm)- HV3 (0.3 mm)- 0.3 mm (bulk) HV3 (4.8 mm) HV3 (1.2 mm) Sample 1, 27 min E 1332 1296 36 20 Sample 2, 27 min E 1443 1407 36 25

Example 6, Impact Toughness Testing of Sample 1 and Sample 2

[0087] The impact toughness of drill bit inserts of Sample 1 and Sample 2 (according to Example 3) in an as-sintered state and following E-treatment was tested using a pendulum hammer impact test. A schematic drawing of the pendulum hammer test set-up is shown in FIG. 10. The test procedure used is as follows:

[0088] A mining insert made according to Example 3 with a dome shaped tip of 5.0 mm radius and a diameter of 10.0 mm is firmly mounted into a holder (A) with only the dome section protruding. On the pendulum (B) a hard counter surface is mounted, depicted in FIG. 15 as a light grey area on the pendulum hammer head. The counter surface used was a polished SNGN plate (h=5.00 mm, 1=19.40 mm, w=19.40 mm) of a hard fine grained hard metal grade having a Vickers hardness (HV30) of approx. 1900.

[0089] When the pendulum is released, the counter surface hits the sample tip. If the sample fails, the impact energy absorbed by the sample AE (in Joules) is, for a given initial pendulum angle, calculated using equation 5.

AE=(m.sub.tot×g×L×(1−cos(α))  (5)

[0090] Where m is the total mass of the pendulum hammer 4.22 kg, g is the gravitational constant 9.81 m/s.sup.2, L is the pendulum hammer length 0.231 m and α is the angle in radians.

[0091] To determine the energy needed to fracture the sample, it is first impacted by the pendulum released from a suitable low angle. The angle is then increased step-wise with a 5 degree step until the sample fails. The sample is impacted once at each impact energy level (angle). A visible crack or spalling is considered as sample failure. The first test starting from the low impact energy level is not counted as valid in the evaluation. In the following tests, used in the evaluation, the angle is lowered by 5 degrees from the angle at which failure was first observed, and subsequently increased again with a finer 3 degree step until failure is reached again. The target result is such that each insert fails at the second angle (impact), however, some of the inserts failed only at the third impact. These were also counted as valid results. Inserts which failed on the first impact were not included in the evaluation. In these tests the counter surface was exchanged every 5-10 impacts. The obtained results for Sample 1 and Sample 2 as a function of different surface treatments are presented in tables 4 and 5.

TABLE-US-00004 TABLE 4 Sample 1 (comparative) Absorbed energy No. of valid Treatment at failure (J) ΔAE (%) tests/samples untreated (OD-ground) 3.5 0 3 27 min E 12.6 261 3

TABLE-US-00005 TABLE 5 Sample 2 (the invention) Absorbed energy No. of valid Treatment at failure (J) ΔAE (%) tests/samples untreated (OD-ground) 3.5 0 3 27 min E 13.8 295 3

[0092] In tables 2 and 3: ΔAE in percentage is calculated as:

ΔAE=((Average AE (Treated)−Average AE (OD−ground))/Average AE (OD−ground))*100)

[0093] where AE is the absorbed energy at fracture.

[0094] The results show that the resistance against failure, measured as the energy needed to fracture the sample, increases more (295%) when comparing a chromium-containing insert that has been E-treated with an insert not containing chromium (261%), the reference level being non-treated (OD-ground) samples.

Example 7, Toughness of Sample 1 and Sample 2

[0095] The toughness of drill bit inserts of Sample 1 and Sample 2 (made according to Example 4) was characterized using the insert compression test, which is an alternative to the pendulum hammer test used in Example 6.

[0096] For each of the materials, Sample 1 and Sample 2, a part of the inserts from the same batch were tested in the as sintered condition, while another part of the inserts were tested following 9 minutes of treatment using the E-method as already described in Example 4.

[0097] The insert compression (IC) test method involves compressing a drill bit insert between two plane-parallel hard counter surfaces, at a constant displacement rate, until the failure of the insert. A test fixture based on the ISO 4506:2017 (E) standard “Hardmetals−Compression test” was used, with cemented carbide anvils of hardness exceeding 2000 HV, while the test method itself was adapted to toughness testing of rock drill inserts. The fixture was fitted onto an Instron 5989 test frame. The loading axis was identical with the axis of rotational symmetry of the inserts.

[0098] The counter surfaces of the fixture fulfilled the degree of parallelism required in the ISO 4506:2017 (E) standard, i.e. a maximum deviation of 0.5 μm/mm. This is of great importance for the test alignment and repeatability of the results. The tested inserts were loaded at a constant rate of crosshead displacement equal to 0.6 mm/min until failure, while recording the load-displacement curve. The test rig and test fixture compliance was subtracted from the measured load-displacement curve before test evaluation. Two inserts were tested per material and treatment. The counter surfaces were inspected for damage before each test. Insert failure was defined to take place when the measured load suddenly dropped by at least 1000 N. Subsequent inspection of tested inserts confirmed that this in all cases coincided with the occurrence of a macroscopically visible crack.

[0099] The material toughness was characterized by means of the total absorbed deformation energy until fracture, denoted as AEIC. AEIC was calculated for each test as the total area under the measured load-displacement curve until fracture. Table 6 shows the average values of AEIC obtained for the Sample 1 and Sample 2 materials in the as sintered state and after 9 minutes of E-treatment, respectively. ΔAEIC, the average percental increase in absorbed energy following the treatment, is also included in the table. The increase was calculated from the average of the absorbed energy values as:

ΔAEIC=((AEIC treated−AEIC as sintered)/AEIC as sintered)*100

TABLE-US-00006 TABLE 6 Absorbed energy in the insert compression test. AEIC AEIC Material (as sintered) (J) (treated 9 min E-method) (J) ΔAEIC (%) Sample 1 0.53 2.99 463 Sample 2 0.68 4.18 511

[0100] It can be seen from the test results that even the short E-method treatment time of 9 minutes resulted in a dramatic increase of the absorbed energy. The effect of the treatment was clearly more pronounced for the chromium containing Sample 2, with ΔAEIC of 511% as compared to the 463% obtained with the chromium-free Sample 1, despite the equal binder phase volume of the two materials.

Example 8, Abrasion Wear Testing

[0101] Drill bit inserts of Sample 1 and Sample 2 according to Example 3 (010 mm OD, spherical front) in an as-sintered state and following E-treatment were tested in an abrasion wear test, wherein the sample tips are worn against a rotating granite log counter surface in a turning operation. The test parameters used were as follows: 200 N load applied to each insert, granite log rpm=280, log circumference ranging from 44 to 45 cm, and a horizontal feed rate of 0.339 mm/rev. The sliding distance in each test was constant at 150 m and the sample was cooled by a continuous flow of water. Each sample was carefully weighed prior to and after the test. Mass loss of one to two samples per material was evaluated after 150 m sliding distance. Sample volume loss for each of the tested materials and different surface treatments, calculated from the measured mass loss and sample density, is presented in table 7.

[0102] The abrasion wear test results clearly show significantly increased wear resistance for the material according to the invention (Sample 2), as compared to the reference material (Sample 1). Further improvement in wear resistance was observed for the inserts that had been subjected to the E-method surface treatment for 27 min.

TABLE-US-00007 TABLE 7 Results as sample wear measured in the abrasion wear test. Mass loss of Volumetric wear Average each specimen Density of each specimen volumetric wear Sample material Treatment (g) (g/cm.sup.3) (mm.sup.3) (mm.sup.3) Sample 1, As sintered 0.0078 15.10 0.517 0.573 comparative dome 0.0095 0.629 Sample 1, 27 min E 0.0071 15.10 0.470 0.470 comparative 0.0071 0.470 Sample 2, As sintered 0.0043 15.00 0.287 0.293 invention dome 0.0045 0.300 Sample 2, 27 min E 0.0034 15.00 0.227 0.217 invention 0.0031 0.207