CN102942366B - Preparation method of Al-Mg-B ceramic material - Google Patents

Preparation method of Al-Mg-B ceramic material Download PDF

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CN102942366B
CN102942366B CN201210423051.6A CN201210423051A CN102942366B CN 102942366 B CN102942366 B CN 102942366B CN 201210423051 A CN201210423051 A CN 201210423051A CN 102942366 B CN102942366 B CN 102942366B
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powder
boron
pressure
block
magnalium
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CN102942366A (en
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刘雯
闫建新
温卫中
王强
苗洋
孟庆森
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Taiyuan University of Science and Technology
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Abstract

The invention relates to a preparation method of an Al-Mg-B ceramic material, characterized by using aluminium powder, magnesium powder and boron powder as raw materials, annealing boron powder, preparing powder in proportion, conducting machinery alloying, conducting pre-press molding, conducting electric field activation, and conducting high temperature pressure sintering to obtain an Al-Mg-B ceramic block. According to the invention, the Al-Mg-B ceramic block has good microstructure density, a fracture toughness of 3MPa.m<0.5>, and a surface friction coefficient of 0.45-0.55; the preparation method has the advantages of advanced process, abundant and accurate data, safety and reliability, low energy consumption, and no environmental pollution, and is an ideal method for preparing the Al-Mg-B ceramic material.

Description

A kind of preparation method of magnalium boron stupalith
Technical field
The present invention relates to a kind of preparation method of magnalium boron stupalith, belong to the preparation of special cermacis matrix material and the technical field of application.
Background technology
Magnalium boron stupalith has the features such as hardness is high, wear resisting property good, chemical stability is good, uses, but because the toughness of magnalium boron material is lower, limited its range of application in the mechanical means of the military equipment of being everlasting and strong mechanical performance.
At present, the method for preparing magnalium boron stupalith has mechanical alloying hot pressing sintering method, heat treating process, crystallization sedimentation, metal-salt preparation method; Mechanical alloying hot pressing sintering method power consumption is high, hardened steel ball causes when ball milling iron pollution is large, complex technical process, difficult control; Heat treating process power consumption is high, cost is high, easily introduce impurity, microhardness is low; Although crystallization sedimentation and metal-salt preparation method purity are high, also can avoid raw material due to high temperature long heat treatment generate dephasign, consume energy high, the cycle is long, cost is high; Although above method also can be prepared magnalium boron stupalith, there is many technical deficiencies and drawback.
Summary of the invention
goal of the invention
The object of the invention is the deficiency for background technology, the method that adopts electric field-activate to combine with pressure assisted sintering is prepared magnalium boron stupalith, to increase substantially the mechanical property of magnalium boron stupalith, expands the range of application of magnalium boron stupalith.
technical scheme
The chemical substance material that the present invention uses is: boron powder, magnesium powder, aluminium powder, dehydrated alcohol, argon gas, it is as follows that it prepares consumption: with gram, milliliter, centimetre 3for measure unit
Aluminium powder: Al powder granule diameter≤2 μ m, 0.4185g ± 0.0001g
Magnesium powder: Mg powder granule diameter≤74 μ m, 0.3609g ± 0.0001g
Boron powder: B powder granule diameter≤60 μ m, 2.0646g ± 0.0001g
Dehydrated alcohol: C 2h 5oH 100mL ± 1mL
Argon gas: Ar 100000cm 3± 100cm 3
Preparation method is as follows:
(1) selected chemical substance material:
The chemical substance material that preparation is used will carry out selected, and carries out quality purity control:
Aluminium powder: solid powder 99.95%
Magnesium powder: solid powder 99.99%
Boron powder: solid powder 99%
Dehydrated alcohol: liquid liquid 99%
Argon gas: gaseous state gas 97%
(2) boron powder vacuum annealing
Boron powder 2.0646g ± 0.0001g is placed in to quartz container, is then placed in vacuum annealing furnace and anneals, 1500 ℃ of annealing temperatures, soaking time 120min, vacuum tightness 10Pa, makes boron powder crystal after annealing;
(3) join powder
In the glove box that passes into argon gas, prepare aluminium powder, magnesium powder, boron powder one-tenth mixing magnalium boron powder;
Figure 375835DEST_PATH_IMAGE001
the aluminium powder of airtight package, magnesium powder, boron powder are placed in respectively to glove box, ball grinder is placed in to glove box, and airtight;
Figure 401560DEST_PATH_IMAGE002
extract air in glove box, make pressure in case reach 1 × 10 -1pa;
Figure 917861DEST_PATH_IMAGE003
in case, input argon gas, argon gas input speed 20cm 3/ min; Making the interior pressure of case identical with outside atmosphere pressure, is a standard atmospheric pressure, and constant;
Figure 422486DEST_PATH_IMAGE004
take aluminium powder 0.4185g, magnesium powder 0.3609g, boron powder 2.0646g, be in mass ratio: aluminium: magnesium: boron=1.16: 1: 5.72;
Figure 888102DEST_PATH_IMAGE005
aluminium powder, magnesium powder, boron powder are put into ball grinder, become magnalium boron powder mix, then pack zirconium oxide abrasive ball into, mill ball: powder mix=10: 1, and encapsulate with paraffin;
(4) magnalium boron powder mix mechanical alloying
The mechanical alloying of magnalium boron powder mix is carried out in ball mill, is to complete under the grinding of zirconium oxide abrasive ball;
Figure 960095DEST_PATH_IMAGE001
the ball grinder that magnalium boron powder mix and zirconium oxide abrasive ball are housed is packed on ball mill, carry out ball milling;
Figure 776741DEST_PATH_IMAGE002
open ball mill, drum's speed of rotation is 250r/min, Ball-milling Time 10h, and by collision, the crush and grind of zirconium oxide abrasive ball, there is moulding distortion, fracture, seam in magnalium boron powder mix particle, and phase mutual diffusion between atom, forms even mixed powder;
(5) pre-molding
Figure 513753DEST_PATH_IMAGE001
prefabricated graphite jig, graphite jig is open-close type, and die cavity is round shape, and in die cavity, graphite cushion block is established in bottom, and graphite briquetting is established on top;
Figure 348722DEST_PATH_IMAGE002
magnalium boron powder mix is added in graphite jig, and magnalium boron powder mix is placed between graphite cushion block and graphite briquetting;
Figure 778567DEST_PATH_IMAGE003
graphite jig is placed on vertical pressing machine and carries out presuppression, and pressing machine pressure is 15MPa, and press time 15s becomes magnalium boron block after presuppression;
(6) the synthetic sintering of magnalium boron stupalith
The synthetic sintering of magnalium boron stupalith block carries out in vertical sintering oven, under heating, pressurization, vacuum state, completes;
Figure 816930DEST_PATH_IMAGE001
the graphite jig that magnalium boron block is housed is placed on the worktable in vertical sintering oven, and worktable is copper electrode, and top briquetting is also copper electrode, vertically exerts pressure;
Figure 170682DEST_PATH_IMAGE002
close sintering oven, and airtight;
Figure 814153DEST_PATH_IMAGE003
open vacuum pump, extract furnace air, make pressure in stove reach 10Pa;
Figure 211636DEST_PATH_IMAGE004
power supply in opening sintering furnace, and heating, make 600 ℃ of stove Nei Wenduda
Figure 940558DEST_PATH_IMAGE006
2 ℃, heating graphite jig and interior magnalium boron block thereof;
Figure 206323DEST_PATH_IMAGE005
the pressure motor on opening sintering furnace top, and by copper electrode pressure block, the magnalium boron block in mould is exerted pressure, pressure is 20MPa, time 2min exerts pressure;
Figure 766617DEST_PATH_IMAGE007
continue to make temperature in stove to rise to 1500 ℃ 2 ℃, continue heating graphite jig and magnalium boron block;
Figure 800487DEST_PATH_IMAGE008
the pressure that continues to increase sintering oven upper pressure motor and copper electrode pressure block, makes pressure reach 60MPa, at 1500 ℃, under 60MPa, keeps 15min, makes it moulding;
Figure 745309DEST_PATH_IMAGE009
close heating power supply, make graphite jig and magnalium boron block cool to 25 ℃ of room temperatures with the furnace;
closing vacuum pump, make the interior pressure of stove identical with outside atmosphere pressure, is a standard atmospheric pressure;
Figure 853391DEST_PATH_IMAGE011
opening sintering furnace, closes and adds Medium-voltage Motor, takes out graphite jig and interior magnalium boron block thereof;
Open graphite jig, take out magnalium boron block, be magnalium boron stupalith;
(7) detect, analyze, characterize
Pattern, color and luster, composition, chemical physics performance, the mechanical property of the magnalium boron stupalith to preparation detect, analyze, characterize;
Carry out material phase analysis with x-ray instrument;
Carry out morphology analysis with JOEL scanning electron microscope;
Carry out ultimate analysis by energy dispersive spectrometry;
Carry out micro area structure analysis with JEOL-2010 type high-resolution-ration transmission electric-lens;
By the microhardness of HVS-1000A microhardness machine measure sample;
With frictional wear instrument measurement frictional coefficient;
Conclusion: magnalium boron stupalith is black, and metallographic structure compactness is good, magnalium boron AlMgB 14quality purity reaches 97%, 3% and is converted into spinel; Hardness reaches 27.2GPa, and mean density is 2.62g/cm 3, fracture toughness property reaches 3MPam 0.5, skin friction coefficient is 0.45 ~ 0.55;
(8) product stock
The magnalium boron stupalith block of preparation is packed with soft material, is stored in cool place, dry, clean environment, 20 ℃ of storing temps, relative humidity≤10%.
beneficial effect
The present invention has obvious advance compared with background technology, to adopt aluminium powder, magnesium powder, boron powder to do raw material, anneal, join in proportion powder, mechanical alloying, pre-molding, high-temperature pressurizing sintering through boron powder, make magnalium boron stupalith block, magnalium boron stupalith block metallographic structure compactness is good, hardness reaches 27.2GPa, and mean density is 2.62g/cm 3, fracture toughness property reaches 3MPam 0.5, skin friction coefficient is 0.45 ~ 0.55, this preparation method's technique advanced person, and informative data is accurate, consumes energy low, free from environmental pollution, is the very good method of preparing magnalium boron stupalith.
Accompanying drawing explanation
Fig. 1 is the heating of magnalium boron stupalith, pressurization, sintering state figure
Fig. 2 is magnalium boron stupalith block square section metallographic structure shape appearance figure
Fig. 3 is the X ray diffracting spectrum of magnalium boron stupalith block
Fig. 4 is the TEM picture of magnalium boron stupalith block
Fig. 5 is A and the B electron diffration by crystals style figure in Fig. 4
Shown in figure, list of numerals is as follows:
1, sintering oven, 2, stove seat, 3, top cover, 4, copper electrode worktable, 5, copper electrode pressure block, 6, pressure motor, 7, vacuum pump, 8, viewing window, 9, graphite jig, 10, graphite cushion block, 11, graphite briquetting, 12, magnalium boron block, 13, movable rack, 14, electric control box, 15, display screen, 16, pilot lamp, 17, vacuum pump modulator, 18, Heating temperature modulator, 19, pressure motor modulator, 20, wire, 21, copper electrode modulator.
Embodiment
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, be the heating of magnalium boron stupalith, pressurization, sintering state figure, each portion position, annexation want correct, proportioning according to quantity, according to the order of sequence operation.
The value of the chemical substance that preparation is used is to determine by the scope setting in advance, with gram, milliliter, centimetre
Figure 353642DEST_PATH_IMAGE012
for measure unit.
The synthetic sintering of magnalium boron stupalith carries out in vertical sintering oven, under vacuum, heating, pressurization, sintering state, completes;
Sintering oven is vertical, sintering oven 1 bottom is stove seat 2, top is top cover 3, be provided with pressure motor 6 on top cover 3 tops, be provided with copper electrode worktable 4 at sintering oven 1 inner bottom part, the vertical graphite jig 9 of putting on copper electrode worktable 4, graphite jig 9 peripheries are fixed by movable rack 13, put graphite cushion block 10 at graphite jig 9 inner bottom parts, be magnalium boron block 12 on graphite cushion block 10 tops, pushed down by graphite briquetting 11 on magnalium boron block 12 tops, pushed down by copper electrode pressure block 5 on graphite briquetting 11 tops, copper electrode pressure block 5 tops connect the pressure motor 6 on top cover 3 tops, be provided with vacuum pump 7 at the right lower quadrant of sintering oven 1, be provided with viewing window 8 at the upper left quarter of sintering oven 1, be provided with electric control box 14 in the left side of sintering oven 1, on electric control box 14, be provided with display screen 15, pilot lamp 16, vacuum pump modulator 17, Heating temperature modulator 18, pressure motor modulator 19, copper electrode modulator 21, electric control box 14 connects with sintering oven 1 by wire 20.
Shown in Fig. 2, for magnalium boron stupalith block square section metallographic structure shape appearance figure, can be observed two kinds of different phases in figure, black region comprises Al, Mg and B element, is AlMgB 14phase; Light gray zones comprises Al, Mg and O element, is spinel MgAl 2o 4phase, O, from initial powder and mechanical milling process, shows AlMgB in figure 14as matter distribution even compact.
Shown in Fig. 3, be magnalium boron stupalith block X-ray diffraction intensity collection of illustrative plates, ordinate zou is diffracted intensity, and X-coordinate is diffraction angle 2 θ, AlMgB 14: MgAl 2o 4peak rate ratio be 6.5, explanation reacts completely, and obtains required thing phase AlMgB 14, product in 2 θ=40.69 °, 42.2 °, 13.89 ° located diffraction peak, these peaks are conventionally at orthogonal AlMgB 14in structure, exist, all the other impurity phases are MgAl 2o 4, MgAl 2o 4come from the oxygen existing in initial feed and mechanical milling process, Al promotes mass transport, the excess of aluminum that adds in advance.
Shown in Fig. 4, be the TEM picture of magnalium boron stupalith block, in figure, two crystal are high-visible, arrow A indication crystal is great majority, spreads all over whole sample, has shown to generate more A crystal, the crystal of arrow B indication distributes seldom, by electron diffraction pattern recognition structure, shows that A is AlMgB 14crystal, B is MgAl 2o 4crystal.
Shown in Fig. 5, be the A in Fig. 4, B electron diffration by crystals style figure, known in figure: (a), zone axis is parallel to [1 1 1], with digital 4,5 and 6 Miller indices that mark diffraction spot be respectively
Figure 774259DEST_PATH_IMAGE013
, , , measure spot spacing by gage, then calculate d value according to camera constant, be respectively d 1=0.63774, d 2=0.50871, d 3=0.47444; Approach AlMgB by calculating lattice parameter 14the theoretical value of crystal; Can confirm that thus crystal A is the AlMgB of an orthohomic lattice 14; (b) Miller indices of spot 1,2 and 3 are respectively
Figure 399691DEST_PATH_IMAGE016
, measure spot spacing by gage, then calculate d value according to camera constant, be respectively d 1=0.46667; d 2=0.46667; d 3=0.40415; Approach MgAl by calculating lattice parameter 2o 4the theoretical value of crystal (spinel); Can confirm that thus crystal B is the MgAl of face-centered cubic lattice 2o 4spinel.

Claims (2)

1. a preparation method for magnalium boron stupalith, is characterized in that: the chemical substance material of use is: boron powder, magnesium powder, aluminium powder, dehydrated alcohol, argon gas, it is as follows that it prepares consumption: with gram, milliliter, centimetre 3for measure unit
Aluminium powder: Al powder granule diameter≤2 μ m, 0.4185g ± 0.0001g
Magnesium powder: Mg powder granule diameter≤74 μ m, 0.3609g ± 0.0001g
Boron powder: B powder granule diameter≤60 μ m, 2.0646g ± 0.0001g
Dehydrated alcohol: C 2h 5oH 100mL ± 1mL
Argon gas: Ar 100000cm 3± 100cm 3
Preparation method is as follows:
(1) selected chemical substance material:
The chemical substance material that preparation is used will carry out selected, and carries out quality purity control:
Aluminium powder: solid powder 99.95%
Magnesium powder: solid powder 99.99%
Boron powder: solid powder 99%
Dehydrated alcohol: liquid liquid 99%
Argon gas: gaseous state gas 97%
(2) boron powder vacuum annealing
Boron powder 2.0646g ± 0.0001g is placed in to quartz container, is then placed in vacuum annealing furnace and anneals, 1500 ℃ of annealing temperatures, soaking time 120min, vacuum tightness 10Pa, boron powder crystal after annealing;
(3) join powder
The preparation of aluminium powder, magnesium powder, boron powder is carried out in glove box, under argon shield, completes;
1. airtight package aluminium powder, magnesium powder, boron powder, be placed in respectively glove box, and ball grinder is placed in to glove box, and airtight;
2. extract air in glove box, make pressure in case reach 1 × 10 -1pa;
3. in case, input argon gas, argon gas input speed 20cm 3/ min; Making the interior pressure of case identical with outside atmosphere pressure, is a standard atmospheric pressure, and constant;
4. take aluminium powder 0.4185g, magnesium powder 0.3609g, boron powder 2.0646g, be in mass ratio: aluminium: magnesium: boron=1.16: 1: 5.72;
5. aluminium powder, magnesium powder, boron powder are put into ball grinder, become magnalium boron powder mix, then pack zirconium oxide abrasive ball into, mill ball: powder mix=10: 1, and encapsulate with paraffin;
(4) magnalium boron powder mix mechanical alloying
The mechanical alloying of magnalium boron powder mix is carried out in ball mill, is to complete under the grinding of zirconium oxide abrasive ball;
1. the ball grinder that magnalium boron powder mix and zirconium oxide abrasive ball are housed is packed on ball mill, carry out ball milling;
2. open ball mill, drum's speed of rotation is 250r/min, Ball-milling Time 10h, and by collision, the crush and grind of zirconium oxide abrasive ball, there is moulding distortion, fracture, seam in magnalium boron powder mix particle, and phase mutual diffusion between atom, forms even mixed powder;
(5) pre-molding
1. prefabricated graphite jig, graphite jig is open-close type, and die cavity is round shape, and in die cavity, graphite cushion block is established in bottom, and graphite briquetting is established on top;
2. magnalium boron powder mix is added in graphite jig, magnalium boron powder mix is placed between graphite cushion block and graphite briquetting;
3. graphite jig is placed on vertical pressing machine and carries out presuppression, pressing machine pressure is 15MPa, and press time 15s becomes magnalium boron block after presuppression;
(6) the synthetic sintering of magnalium boron stupalith
The synthetic sintering of magnalium boron stupalith block carries out in vertical sintering oven, under heating, pressurization, vacuum state, completes;
1. the graphite jig that magnalium boron block is housed is placed on the worktable in vertical sintering oven, worktable is copper electrode, and top briquetting is also copper electrode, vertically exerts pressure;
2. close sintering oven, and airtight;
3. open vacuum pump, extract furnace air, make pressure in stove reach 10Pa;
4. power supply in opening sintering furnace, and heating, make 600 ℃ ± 2 ℃ of stove Nei Wenduda, heating graphite jig and interior magnalium boron block thereof;
5. the pressure motor on opening sintering furnace top, and by copper electrode pressure block, the magnalium boron block in mould is exerted pressure, pressure is 20MPa, time 2min exerts pressure;
6. continue to make temperature in stove to rise to 1500 ℃ ± 2 ℃, continue heating graphite jig and magnalium boron block;
7. the pressure that continues to increase sintering oven upper pressure motor and copper electrode pressure block, makes pressure reach 60MPa, at 1500 ℃, under 60MPa, keeps 15min, makes it moulding;
8. close heating power supply, make graphite jig and magnalium boron block cool to 25 ℃ of room temperatures with the furnace;
9. closing vacuum pump, make the interior pressure of stove identical with outside atmosphere pressure, is a standard atmospheric pressure;
10. opening sintering furnace, closes and adds Medium-voltage Motor, takes out graphite jig and interior magnalium boron block thereof;
Figure FDA0000494408260000031
open graphite jig, take out magnalium boron block, be magnalium boron stupalith;
(7) detect, analyze, characterize
Pattern, color and luster, composition, chemical physics performance, the mechanical property of the magnalium boron stupalith to preparation detect, analyze, characterize;
Carry out material phase analysis with x-ray instrument;
Carry out morphology analysis with JOEL scanning electron microscope;
Carry out ultimate analysis by energy dispersive spectrometry;
Carry out micro area structure analysis with JEOL-2010 type high-resolution-ration transmission electric-lens;
By the microhardness of HVS-1000A microhardness machine measure sample;
With frictional wear instrument measurement frictional coefficient;
Conclusion: magnalium boron stupalith is black, and metallographic structure compactness is good, magnalium boron AlMgB 14quality purity reaches 97%, 3% and is converted into spinel; Hardness reaches 27.2GPa, and mean density is 2.62g/cm 3, fracture toughness property reaches 3MPam 0.5, skin friction coefficient is 0.45～0.55;
(8) product stock
The magnalium boron stupalith block of preparation is packed with soft material, is stored in cool place, dry, clean environment, 20 ℃ of storing temps, relative humidity≤10%.
2. the preparation method of a kind of magnalium boron stupalith according to claim 1, is characterized in that: the synthetic sintering of magnalium boron pottery carries out in vertical sintering oven, is in heating under vacuum, and pressurization, completes under sintering state;
Sintering oven is vertical, sintering oven (1) bottom is stove seat (2), top is top cover (3), be provided with pressure motor (6) on top cover (3) top, be provided with copper electrode worktable (4) at sintering oven (1) inner bottom part, at the upper vertical graphite jig (9) of putting of copper electrode worktable (4), graphite jig (9) periphery is fixing by movable rack (13), put graphite cushion block (10) at graphite jig (9) inner bottom part, be magnalium boron block (12) on graphite cushion block (10) top, pushed down by graphite briquetting (11) on magnalium boron block (12) top, pushed down by copper electrode pressure block (5) on graphite briquetting (11) top, copper electrode pressure block (5) top connects the pressure motor (6) on top cover (3) top, be provided with vacuum pump (7) at the right lower quadrant of sintering oven (1), be provided with viewing window (8) at the upper left quarter of sintering oven (1), be provided with electric control box (14) in the left side of sintering oven (1), on electric control box (14), be provided with display screen (15), pilot lamp (16), vacuum pump modulator (17), Heating temperature modulator (18), pressure motor modulator (19), copper electrode modulator (21), electric control box (14) connects with sintering oven (1) by wire (20).
CN201210423051.6A 2012-10-30 2012-10-30 Preparation method of Al-Mg-B ceramic material Expired - Fee Related CN102942366B (en)

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CN103342575B (en) * 2013-07-11 2015-01-21 太原理工大学 Reaction diffusion connecting method of superhard material aluminum magnesium boron-titanium diboride and metal
CN104591769B (en) * 2014-12-30 2016-05-25 广东工业大学 Toughness reinforcing enhancing pottery of a kind of magnalium boron and preparation method thereof
CN108726527A (en) * 2018-06-06 2018-11-02 王岚 A kind of AlMgB14/ graphene composite powder material and preparation method thereof
CN111454062B (en) * 2019-01-22 2022-03-08 中国科学院上海硅酸盐研究所 AlMgB14Preparation method of ceramic material powder
CN115246739A (en) * 2022-01-12 2022-10-28 扬州工业职业技术学院 Aluminum-magnesium-boron-zirconium diboride two-phase composite material and preparation method thereof
CN115872778B (en) * 2022-12-14 2023-12-01 中国科学院兰州化学物理研究所 Method for realizing lubrication and ultralow abrasion of Wen Youliang at temperature of more than 900 DEG C

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