前苏联专利SU1308193A3 Hot compaction ceramics for cutting tool

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专利摘要:
PURPOSE:To produce the sintered material for cutting tools having excellent wear resistance, strength and heat resistance, by sintering BN of cubic system using carbides, nitrides, borides or silicides of the specified metals as the binding phase.
公开号:SU1308193A3
申请号:SU772557750
申请日:1977-12-20
公开日:1987-04-30
发明作者:Хара Акио；Язу Судзи
申请人:Сумитомо Электрик Индастриз Лтд (Фирма)；
IPC主号:

专利说明:

eleven
The invention relates to the field of producing highly hard ceramic materials for cutting tools. A ceramic material based on boron carbide of cubic modification and 30% carbide of a heat-resistant metal (titanium, tantalum, tungsten or a mixture thereof) with a metallic binder material is known, and the particle size of boron nitride exceeds 80 μm The material has a structure composed of relatively large grains of boron nitride, directly related to each other.
The material, when used as a cutting tool, does not have sufficient resistance when cutting high-hardened steel.
The aim of the invention is to increase wear resistance.
This goal is achieved due to the fact that hot pressing ceramics for cutting and treating metals containing boron nitride of cubic or wurtdite modification and refractory carbide and / or nitride, or boride or silicide of a transition metal from the group: Ti, Zr, Hf, V, Nb, Ta, W, contains boron nitride with a particle size of ilO μm, dispersed in the matrix of refractory carbide and / or nitride, or boride, or silicide of the specified transition metal in the following ratio of components, OBL:
Boron nitride with a particle size of 10 microns 10-80 Refractory carbide and / or nitride, or boride, or a transition metal silicide from the group: Ti, Zr, Hf, V, Nb, Ta, W20-90

In addition, it contains carbide
When used, for example. The composition nitrides (where Me is Ti, Zr, Hf, V, Nb, Ta, W, ax means the existence of either a vacancy or an extra atom) it was found that some nitrides with a value of x in a limited range (x 0.97) exhibit lunguyu degree sintering. A fine powder of BN particles of a few microns, 35 or less, contains a relatively large amount of oxygen, most of which is usually present as hydroxide or the like. When this hydroxide compound is heated, it is decomposed to form gases. If the material to be sintered is not fully compacted, it is not difficult to remove the gases from the system. However, during sintering under ultrahigh / or nitride of a transition metal with certain pressures, as in the invention,
Mea
1iX where Me is transition metal
A - C and / or Nj 1 + x 0.97. In order to give hot pressing to the ceramics on the basis of cubic BN, the properties required for the tool can be used to remove gases from the system. In this case, the material is usually pre-degassed, as is known from powder metallurgy. However, if it is not possible to use high temperatures during degassing, as in this case, a problem arises. Thus, heating temperatures are limited due to the re-conversion of the machining cubic, for example, for a cutting tool, the necessary BN in the form of low pressure with a nitrous binding material that has boron boron. .
more high thermal conductivity. The process of degassing fine heat resistance, hardness, seam soldering is carried out as follows.
five
resistance to abrasion, viscosity, anti-reactivity to the workpiece, than these known binding metals, such as kolbat.
In the invention, carbides, nitrides, carbonitrides, borides, and silicides of metals of the transition groups IVA (Ti, Zr, llf,), Va (V, Nb, Ta, W) of the periodic table are selected as binder materials that meet these requirements. , mixtures thereof, and compounds of their solid solutions. These compounds mainly possess high values of hardness, welding temperature and thermal conductivity, close in magnitude to the thermal conductivity of metals. It is established that the lower limit of the content of cubic (wurtzite) 0 BN is 10%. With less of its content, ceramics do not show the properties inherent in cubic BN in the instrument; with the content of the latter more than 80%, it is impossible to obtain the material of the required structure.
When used, for example. The composition nitrides (where Me is Ti, Zr, Hf, V, Nb, Ta, W, ax means the existence of either a vacancy or an extra atom) it was found that some nitrides with a value of x in a limited range (x 0.97) exhibit lunguyu degree sintering. A fine powder of BN particles of a few microns 5 or less contains relatively large amounts of oxygen, most of which is usually present as hydroxide or the like. When this hydroxide compound is heated, it is decomposed to form gases. If the material to be sintered is not fully compacted, it is not difficult to remove the gases from the system. However, when sintering under ultrahigh3
0
0
50
It is possible to remove gases from the system. In this case, the material is usually pre-degassed, as is known from powder metallurgy. However, if it is not possible to use high temperatures during degassing, as in this case, a problem arises. Thus, heating temperatures are limited due to the reconversion of cubic BN to the form of low boron nitride pressure. .
Physically adsorbed gas and water are first removed at low temperatures. The chemically adsorbed gas and oxide hydrates are then cleaved. Finally, oxides remain. Due to the fact that the cubic BN is stable at temperatures below, it can be preheated to at least this point. Therefore, if the pre-degassing treatment is carried out, the remaining gas KONOIO additives are in the form of oxides. However, since it is necessary for the pressed ceramics to contain as few gaseous components as possible, it is preferable to remove water and hydrogen using pretreatment.
In the process described, all materials of the invention are subjected to vacuum degassing at a pressure below 10 mm Hg. at temperatures over 10 min.
The reasons why it is possible to obtain a better pressed ceramics with the addition of N. are as follows.
Oxides in the form of BjOj exist on the surfaces of cubic BN powder even after the specified degassing treatment. When it is V20z, the Me part, corresponding to (ix) from MeN,, reacts
., + + ZMEO,
no gas is formed and Me has the same crystal structure as MeN, whereby a solid solution is formed. This may be the reason why nitrides Ti, Zr and Hf, depicted as MeN, (, exhibit a higher degree of sintering.
These considerations apply not only to nitrides, but also to carbides of the formula, carbonitrides of the formula Me (C, N) + ;, their mixtures, as well as compounds of their solid solutions.
It is established that when the compounds Ti, Zr, Hf, V, Mb and Ta, W formulas, MeC.jj + y and Me (C, N). have values (1 + x) less than 0.97, they exhibit an excellent degree of sintering.
In addition, various materials were obtained from, the value of (1 + x) to which varied over a wide range. Each of the materials were mixed
g 10. f5
20
25
30 35
40
45
0
55
with cubic BN and sintered at-high temperatures under high pressure in order to obtain hot-pressed ceramics. As a result of studying the properties of each pressed ceramic, it was found that in all cases densely-pressed pressed ceramics has a high hardness, and the TiN lattice constant in the pressed ceramics were blessed than the constant TiN lattice in the powder material,
Example 1, Cubic BN Powder with an average particle size of 7 μm and TiNpg powder. with an average particle size of 1 micron, they were thoroughly mixed at a volume ratio of 60:40 in a mortar. The powder mixture after adding: a weight of 2 wt%, camphor, based on the total weight of the mixture, was molded into an unfired compact with an outer diameter of 10 mm and a height of 1.5 mm. The unfired compact was placed in a stainless steel capsule. The capsule was heated at 10 mm Hg for 20 minutes in vacuum, for degassing in a vacuum oven. The capsule is placed in an ultra-high pressure-type apparatus using pyrophyllite as the pressurized medium, and a graphite pipe as the heater. The space between the sample and the heater is filled with sodium chloride. First, the pressure is raised to 55 kbar, then the temperature is raised to 1400 ° C. After lifting for 30 minutes, the temperature is reduced and the pressure is gradually removed to obtain hot pressing ceramics according to the invention with an outer diameter of 10 mm and a thickness of 1 mm.
The ceramics of the hot pressing thus obtained are ground with a diamond disc to obtain a flat surface, which is then polished with a diamond, with a paste. As a result of X-ray diffraction analysis, a small amount of TiBj was detected, along with cubic BN and TiN. The average hardness of hot pressing ceramics was 3200 kg / mm (according to the results of a Vickers microhardometer).
Hot pressing ceramics was cut with a diamond cutter into the working end of the cutting tool. The working end was brazed to a steel base. In cutting tests, JiS SNCM9 steel with a hardness of HRC
54 after heat treatment, the tools were cut under the following conditions: cutting speed of 120 m / min, cutting depth of 0.2 mm and feed of O, 12 mm per revolution. The cemented alloy cutting tool of the invention was capable of continuous cutting for 35 minutes before the wear width on the protruding surface of the tool edge reached 0.2 mm.
Example 2 A cubic BN powder with an average particle size of 4 μm and Ti powder (C (, N, 4) O90 °) with an average particle size of 1 μm were mixed at a volume ratio of 70: 30 and molded into hot pressed ceramics as in Example 1.
Hot pressing ceramics was spun off with a diamond disc and brazed to the cemented carbide end of the milling tool.
To test the cutting, a JiS FC 25 steel casting with a width of 80 mm and a length of 300 mm was cut in the longitudinal direction with a cylindrical cutter using a water-soluble cutting oil, under the conditions: cutting speed 500 m / min, cutting depth 1 mm
responsibly. The cutting tests were carried out under the conditions: cutting speed 150 M / 1-GIN, cutting depth 0.5 mm and feed O, 1 mm per revolution, on the rod
5 of thermally refined JiSS45C steel to examine the surface roughness. All cutting tools tested had a cutting edge.
0, with a radius of 0.8 mm. When using cutting tools of samples 3,4 or 5 according to the invention, the roughness of the treated surface was 2-3 µm, but when using cutting tools made of hot pressed ceramics consisting only of TiN and of the usual cemented carbide corresponding to JIS PIO, then the roughness is between 20 and 6 6 and 6 - 12 microns, respectively.
Example 4. A wurtdite BN powder containing 0.7 wt.% Oxygen with an average particle size of less than 2 microns, obtained by the so-called shock wave method, was mixed in a ball mill for 48 hours with a TiNgg powder with an average particle size of 1 µm, containing 18.1 wt.% of nitrogen, in a weight ratio of 60:40,
and feed rate of 2800 mm / min. The cutting of the 1st instrument using acetone as a solvent according to the invention was able to cut through 500 passes.
Example 3. A mixture of cubic BN powder with an average particle size of 4 µm and one of the binding compounds in a volume ratio indicated in Table 1 was molded into an unburnt compact in the same manner as in Example 1.
The unfired compact was then placed in a molybdenum capsule and, after preheating, subjected to sintering using an apparatus.
700 ° C
tel. The powder mixture was molded into an uncompressed compact with an outer diameter of 10 mm and a thickness of 1.5 mm, and then it was placed in an iron cup in the form of a cylinder equipped with a bottom part. The capsule was placed in a vacuum oven and heated for 20 minutes under. pressure of 10 mm Hg for its degassing.
The de-asserted product was placed in an ultra-high pressure machine of the type with pyrophyllite as a press medium and a graphite tube as a heater, at a high pressure, with the temperature between the sample and the heating heated during sintering for 20 minutes, as in Example 1 ,
Each of these ceramics pressing gave a dense structure. The receiver was filled with sodium chloride. First, the pressure was raised to 55 kbar, then the temperature was raised and held at 1200 s for 30 minutes.
After that, the temperature was lowered and prepared either from sample 3, the pressure was gradually removed from the sample, resulting in 4 or from sample 5 obtained above, and to compare two hot-pressing inceramics, according to the invention.
The structure was made of hot pressing ceramics from TiNjjqo powder pressed at T 700 C for 15 min under a pressure of 200 kg / cm and from cemented JiS PIO carbide, respectively. The cutting tests were carried out under the conditions: cutting speed 150 M / 1-GIN, cutting depth 0.5 mm and feed O, 1 mm per revolution, on the rod
of thermally refined JiSS45C steel to examine the surface roughness. All cutting tools tested had a cutting edge.
0.8 mm radius. When using cutting tools of samples 3,4 or 5 according to the invention, the roughness of the treated surface was 2-3 µm, but when cutting tools were used from hot pressing ceramics consisting only of TiN and of conventional cemented carbide corresponding to JIS PIO , then the roughness is between 4 6 and 6 - 12 microns, respectively.
Example 4. A wurtdite BN powder containing 0.7 wt.% Oxygen with an average particle size of less than 2 microns, obtained by the so-called shock wave method, was mixed in a ball mill for 48 hours with a TiNgg powder with an average particle size of 1 µm, containing 18.1 wt.% of nitrogen, in a weight ratio of 60:40,
using acetone as a solution 700 ° C
tel. The powder mixture was molded into an uncompressed compact with an outer diameter of 10 mm and a thickness of 1.5 mm, and then it was placed in an iron capsule in the shape of a cylinder equipped with a bottom part. The capsule was placed in a vacuum oven and heated for 20 minutes under. pressure of 10 mm Hg for its degassing.
The decontaminated product was placed in an ultra-high pressure machine of the type with pyrophyllite as a pressing medium and a graphite tube as a heater, and the pritele was filled with sodium chloride. First, the pressure was raised to 55 kbar, then the temperature was raised and held at 1200 s for 30 minutes.
After that, the temperature was lowered and the pressure was gradually removed, obtaining
55
hot pressing ceramics according to the invention.
The hot-pressed ceramics thus obtained after grinding with a diamond wheel was polished with grinding with diamond paste. The Vickers hardness of the ground surface of the pressed ceramic was AQO kg / mm. An X-ray diffraction pattern of a ground surface gives weak peaks, which can be attributed to TiBj along with peaks corresponding to wurtzite BN and solid solution Ti (N, 0).
Example 5. The same wurtzite BN powder used in Example 4 was mixed with one of the bonding compounds in a specific volume ratio and molded into hot pressing ceramics according to the invention, having a dense structure, maintaining temperature and pressure values for 30 min. Then, the hardness of the hot pressing ceramic was measured. The results are shown in table 2.
20
; T1 (Co, 8C, 0, if) o, 9J. Ti (with 0.5, No, 3) o, 8 nil0.7,) No, 9.
(, Mo 0.1) C 0.9.
(, Wo,) Co, 9.
(Tio, 8, 2 0, 0.4
Example 6. TOT the same powder wurtzite BN, which was used in example 3, was mixed with powder
a higher value than the maximum value for TiN., .. The reason for which the lattice constant changes in the pressed ceramics of the invention is as follows: It is known that there are a large number of atomic voids in Ti and N of the formula TiN / i + , f even if TiN
25
N rt) 0.9
d is a stoichiometric compound. used to obtain the experimental results of Fig. 1, has a greater number of atomic voids N than Ti, in which atomic voids must also be found. Lig.1 of curve A shows the lattice constants of pressed ceramics, which were obtained by sintering powdered TiN | j-j2 containing cubic BN under a pressure of 55 kbar at various temperatures. In this case, the TiN lattices also become higher than in the TiN powder material, due to the treatment with high TeNffiure and pressure. Therefore, the higher the cteneHb of an atomic void, the less constant the Kristapple lattice. The change in the degree of atomic void can occur due to the movement of atom TiC (j | -9s in a volume ratio, indicated by 30 ° y voids within the crystalline lattice in Table 3. of this lattice under the action of
high temperatures and pressures, whereby the void degree is reduced to a certain value.
Figure 1 shows the measurement results by X-ray diffraction.
analysis of TiN lattice constants in kera55 at a determined temperature and pressure of hot pressing, which means that with TiO with the same crystal under a pressure of 55 kbar at different temperatures by mixing 60 vol.% of powdered cubic BN having particles of three different sizes and 40% by volume
(nitrogen content 17.4% in TiN) having an average particle size of 1 μm. In Fig. 1, bright squares show ceramics of cubic BN using particles with an average size of 1 µm, bright triangles of -3 µm, and bright circles. -5 µm, line A shows the lattice constants
tic structure.
Thus, each point plotted in Fig. 1 is a measurement value of hot pressed ceramics that was densely concentrated.
tured and possessed high hardness (о. In the measured range, the TiN lattices in ceramics of the hot pressing according to the invention are higher than the crystalline lattice of both the TiN powder material and the ceramics consisting of TiN. The higher from one TiNp, and the line 50 is the greater the lattice constant, B is the powder lattice constant which usually reaches a constant material.
Permanent lattice material
TiN
0.72
was 4.232 A,
while, in pressed cubic BN and .TiNp ceramics, the TiN permanent lattices (as the matrix for cubic BN) were larger and had
-55th value, and the smaller the particle size of the used powder material of cubic BN, the greater the lattice constant at low temperatures. This is due to the fact that, during sintering, the part that is relatively rich in Ti in the powder mother
W 15 20

81938
a higher value than the maximum value for TiN., .. The reason why the lattice constant in the pressed ceramics of the invention changes varies as follows. It is known that there is a large number of atomic voids in Ti and N of the formula TiN / i +, f even if TiN
25
d is a stoichiometric compound. used to obtain the experimental results of Fig. 1, has a greater number of atomic voids N than Ti, in which atomic voids must also be found. Lig.1 of curve A shows the lattice constants of pressed ceramics, which were obtained by sintering powdered TiN | j-j2 containing cubic BN under a pressure of 55 kbar at various temperatures. In this case, the TiN lattices also become higher than in the TiN powder material, due to the treatment with high TeNffiure and pressure. Therefore, the higher the cteneHb of an atomic void, the smaller the Kristapple lattice constant. The change in the degree of atomic void can occur due to the movement of an atom with a definable temperature and pressure, which was with TiO with the same crystal--
tic structure.
Thus, each point plotted in FIG. 1 is a measurement value of hot pressed ceramics that was densely concentrated.
It is tinted and possesses high hardness (о. In the measured range, the TiN lattices in ceramics of hot pressing according to the invention are higher than the crystalline lattice of both the TiN powder material and the ceramics consisting of TiN. the greater is the lattice constant, which usually reaches a constant
50 the more the lattice constant, which usually reaches a constant
55th value, and the smaller the particle size of the used powder material of cubic BN, the greater the lattice constant at low temperatures. This is due to the fact that, during sintering, the part, which is relatively rich in Ti, in the powder material .9308193
al TiN.,. TiB or TiB npvj is formed by the reaction of TiN and BN, which is the solid component of the pressed ceramic according to the invention, and at the same time N in BN diffuses into 5 matrices, filling the atomic voids comparatively depleted in N in,. In this case, if a finer powder of cubic BN is used, the area of wear resistance becomes larger. tact with the powder, which contributes to the specified reaction at low temperatures. According to the invention, by reacting on contact surfaces between particles of TiN and cubic BN, which is a solid component, it is possible to obtain a very solid
ten
Fig. 2 shows, from the cutting tool with the effect of the BN content obtained by the invention, on the time that the ceramic has worn out.
Thus, the content of the cases 10-80% is about

权利要求:
Claims (1)
[1]
Formula isob
15
1, Ceramics is a hot cutting tool for nitride, boron. Cubic MODIFICATION and torsional and / or nitride, or a transition metal boride from Zr, Hf, V, Nb, Ta, W, due to the fact that wear resistance is Boron nitride with a size of h dispersed in matrix carbide and / or nitride, or a silicide of the specified metal with the following components, vol.%:
densely concentrated pressed ceramics, in which particles of cubic BN are tightly bound together with a matrix of TiN crystals,
Using powder materials with different values (1 + x), it was found that the temperature conditions in which densely concentrated ceramics can be obtained shift to higher values as the value (1 + x) becomes larger. The reason is that the comparative excess of Ti decreases, which is involved in the reaction with particles of cubic BN, as well as the degree of atomic void N as the value (1 + x) becomes larger.
However, if sintering is carried out in an ultra-high pressure device, as in the invention, it is most preferable to carry out the process at lower temperatures, since in this case the service life of the device can be extended and the interaction of hot pressing ceramics with the surrounding material can be reduced.
These results can, in addition, be applied to Ti (C, N) v |,
35 30
Tic
0.97
TiN
0.73
wear resistance.
ten
Fig. 2 shows the wear resistance of the cutting tool with ceramics obtained according to the invention in Fig. 3 — the effect of the BN content of a dense modification on the time during which the ceramics wears by a certain amount.
Thus, the BN content in the range of 10-80% is an area of increased wear resistance.
Invention Formula
wear resistance.
1, Hot pressing ceramics for cutting tools containing nitride, boron. Cubic or wurtzite MODIFICATION and refractory carbide and / or nitride, or boride, or transition metal silicide from the group Ti, Zr, Hf, V, Nb, Ta , W, characterized in that, in order to increase wear resistance, it contains boron nitride with a particle size: 10 μm dispersed in the matrix of refractory carbide and / or nitride, or boride, or silicide of the specified transition metal in the following ratio of components; %:
Boron nitride with a particle size of 10 microns 10-80
Refractory carbide
and / or nitride, or boride, or transition metal silicide from the group Ti, Zr, Hf, V, Nb, Ta, W 20-90
2, Ceramics pop, 1, characterized in that it contains a transition metal carbide and / or nitride
MeA ,.
(where Me is metal; A - C and / or NJ 1 + X 0.97.
Table 1
50
40
1500 1300
eleven
Sample
15 35 35 35 35
TiN, ZrN
we
TaC ZrB
0.73
0.89
0.92
1308193
12 Continuation of table 1
85 65 65 65 65
30 50 50 50 55
1100 1350 1400 1600 1600
table 2
13
TiBAtmpamypa sintering CO 8. 1
130819314
T a b l and c a 3
510 O AOR O DO
Cutting time {myn.) (Rie.
ABOUT
go w bo 80 ioo
The content of wurzitpio BN (volume%} (Riz. 3
Editor M.Kelemes
Compiled by N. Sobolev
Tehred M. Khodanich Proofreader T. Kolb
Order 1644/58 Circulation 588 Subscription
VNIIPI USSR State Committee
for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5
Proizvodstvenno-loligraphicheskoe enterprise, Uzhgorod, Projecto st., 4

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法律状态:

优先权:

申请号 | 申请日 | 专利标题

JP15457076A|JPS573631B2|1976-12-21|1976-12-21|

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