CN106518090A - Sialon ceramic friction welding stirring head and production method thereof - Google Patents
Sialon ceramic friction welding stirring head and production method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of friction welding stirring heads, and discloses a sialon ceramic friction welding stirring head and a production method thereof. The friction welding stirring head is creatively produced from sialon ceramic, the sialon ceramic has good toughness, very high hardness, very high wear resistance and very high high-temperature oxidation resistance, and raw materials of the sialon ceramic have low prices and wide sources. A traditional ceramic technology and high-molecular chemistry are organically combined, a high-molecular polymer polymerization technology is introduced to a ceramic production technology, and a gel injection molding technology is adopted, so compared with other molding technologies, the method disclosed in the invention has the substantial advantages of short production time, low die and device requirements, low cost, and high structure and component designability; the density of the above product is uniform; a green body has a high strength, and is convenient for machining; and the method is especially suitable for realizing near-net-shape forming, realizes small product shape limitation, can be used to produce complex profiled parts, and is universal and economic.
Description
Technical field
The present invention relates to friction welding (FW) stirring-head technical field, more particularly, to a kind of Sialon ceramics friction welding (FW) stirring-head
And preparation method thereof.
Background technology
The fast development of current high performance ship depends not only on the high intensity new diseases such as aluminium alloy, also relies on
The progress of its solder technology.But there is two kinds of different-metal material welding difficult problems of aluminum steel, agitating friction weldering conduct in high speed Aluminium ships
A kind of new solid phase connecting method, it is not substantially by factors such as material physical chemistry performance, mechanical performance and crystal structures
Affect, for the welding of foreign material has great advantage.Therefore, agitating friction weldering is to solve current high-speed ship aluminum steel weldering
Connect the first-selected interconnection technique of a difficult problem.
" heart " of the stirring-head as agitating friction weldering, its material and structure are the cores of agitating friction welding technology.Stirring
Head directly bears the heat load of welding process, power and carries and fretting wear, therefore it is required that the material for manufacturing stirring-head need to have height
Fusing point, intensity, hardness and toughness, good antiwear property and heat-resisting quantity in materials to be welded etc..For aluminum steel is welded, by
It is materials with high melting point in steel, in welding, maximum temperature is up to more than 1000 DEG C.Current conventional stirring head material is mainly tungsten
Sill and cubic boron nitride.But tungsten is expensive, and tungsten is difficult to machining, difficult molding abnormity size element, and stirs
Head is polymorphic structure, therefore tungsten-bast alloy stirring-head manufacturing cost is very high.Cube BN stirring-heads high-temperature stability and wearability
Well, elevated temperature strength and hardness are high, but a manufacture cube BN needs High Temperature High Pressure, and molding abnormity size element is also more difficult.Thus it is vertical
Square BN stirring-heads manufacturing cost is also very high, expensive.Therefore, urgent needss Development of Novel high-performance high temperature resistant agitating friction weldering
Stirring head material and its low cost, controllable standby technology.
Sialon ceramics at high temperature have hardness height, good toughness, creep is little, anti-thermal shock non-oxidizability is strong, the coefficient of expansion is little,
The superior physical and chemical performance such as chemical stability is high, wear-resistant, corrosion-resistant.And its process maturation is controllable, raw material is domestic
Change degree is high, relative inexpensiveness.Therefore, Sialon ceramics is currently to substitute existing high temperature resistant stirring head material, prepares high-performance
The most ideal material system of inexpensive stirring friction welding agitator head.The forming method of Sialon ceramics is mainly heat pressing process at present,
Preparing polymorphic structure stirring-head, to still need to the later stage machining.But Sialon ceramics is hard phase, its processing difficulties and yield rate compared with
It is low, thus Sialon ceramics stirring-head there is also the higher problem of manufacturing cost at present, be badly in need of exploitation Sialon ceramics stirring-head net scale
Very little moulding process is reducing manufacturing cost.
The content of the invention
The technical problem to be solved in the present invention is a kind of Sialon ceramics friction welding (FW) stirring-head for the deficiencies in the prior art
And preparation method thereof.
The purpose of the present invention is achieved by the following technical programs：
A kind of process for preparing Sialon ceramics friction welding (FW) stirring-head is provided, is comprised the following steps：
S1. prepare Sialon ceramics powder：According to molecular formula Si of Sialon ceramics4Al2O2N6Calculate and weigh weighing corresponding
Si3N4, AlN and Al2O3, add Y2O3After obtain batch mixing, gained batch mixing is carried out into ball milling, then dried, seal；
S2. gel casting forming：
S21. premixed liquid is configured, the premixed liquid includes monomer, cross-linking agent and dispersant, respectively N- methylols acryloyl
Amine, N, N- dimethyl-ethylenediamines, ammonium polyacrylate；
S22. step S21 premixed liquid is added in the Sialon ceramics powder obtained by step S1, carries out ball milling, obtain required injection molding
Slurry；
S23. injection molding slurry obtained by step S22 is added into ammonium persulfate solution and tetramethylethylenediamine Jing after froth in vacuum,
Polymorphic structure stirring-head mould is injected after being uniformly mixed, after normal temperature cure molding, process is dried；
S3. defat and sintering：S2 prepared base substrate is put into nitrogen atmosphere stove carries out temperature programming, first completes defat, then
Using two-step method molding, the Sialon ceramics friction welding (FW) stirring-head is obtained.
Molecular formula Si is adopted in step S14Al2O2N6Sialon ceramics reason be low Z values series (Z=0.3, Z=0.6)
β-Sialon Y is easily formed in sintering process2SiAlO5N (B phases), Y2SiAlO5N (B phases) is unfavorable to the toughness of material, must be logical
Cross control technological parameter and avoid Y2SiAlO5The generation of N (B phases), (Z=3, β-Sialon 4) are in sintering process for high Z values series
Si is formed easily2Al3O7N and AlN polytypes, its mechanical property to β-Sialon materials are unfavorable.
The present invention creatively prepares friction welding (FW) stirring-head as raw material using Sialon ceramics, and Sialon ceramics has preferable
Toughness, very high hardness and wearability, and very high high-temperature oxidation resistance, and the Sialon ceramics prices of raw materials are cheap,
Wide material sources.
Traditional ceramicses technique and polymer chemistry are also combined by the present invention, by the polymerization side of high molecular polymer
Method is substituted in the preparation technology of ceramics, using gel injection molding and forming technology, this method compared with other moulding processs, with aobvious
The advantage of work：Preparation time is short and not high to mould and equipment requirements makes which with low cost；Structure and component designability are strong；System
The even density of product；Green strength is high, is easy to machining；Particularly be capable of achieving near-net-shape, article shape be limited it is little,
Complex Different Shape part can be prepared, also with versatility and the features such as economy.
Preferably, dried described in step S1 is that 6～10h is dried in 80 DEG C of baking ovens.
Preferably, Y described in step S12O3For 3～6wt%, Y2O3It is as stabilizer, further in addition Sialon ceramics powder
Improve material property.
Preferably, ball milling described in step S1 is further comprising the steps of：
S11. by batch mixing, mill ball and ball-milling medium according to mass ratio 1:1.5:2 load in ball grinder；The mill ball choosing
Different size of corundum, the ball-milling medium is used to select dehydrated alcohol, the ball grinder to select agate jar；
S12. the ball grinder for installing sealing is put into into 20～24h of ball milling in planetary ball mill.
Sialon ceramics Powder Particle Size can be allowed lower using planetary ball mill, beneficial to follow-up process.
Preferably, N hydroxymethyl acrylamide described in step S21 is 15～20wt%, the N, and N- dimethyl-ethylenediamines are
9～10wt%, the ammonium polyacrylate are 5～6vol%.
Preferably, the ammonium polyacrylate is dissolved in deionized water, and is 9～10 with ammonia regulation pH value, with potentiation
Effect.
Preferably, ball milling described in step S22 adds the Y of 8～10wt% in being additionally included in mixed liquor2O3With 5～7%wt%
Al2O3Used as sintering aid, Ball-milling Time is 4～6h.
Preferably, ammonium persulfate solution described in step S23 be 10～12wt%, the tetramethylethylenediamine be 5～
6wt%.
Preferably, dried described in step S23 is to be dried to quality no longer to change in 50～80 DEG C of baking oven, low temperature
Injection molding dead size moulding process, its process is simple, parameter are controllable, easily prepare Complex Different Shape size stirring-head, and semifinished product precision is high, plus
Spare time amount is few, substantially reduces the preparation cost of stirring-head and its cost of through engineering approaches application.
Preferably, defat described in step S3 is referred under 0.05～0.1Mpa nitrogen atmospheres, with the heating rate of 1 DEG C/min
Defat is completed to 800～900 DEG C；It is 0.1～2.1MPa that the two-step method refers to that green compact are placed on nitrogen pressure by the first step,
1150 DEG C～1850 DEG C of temperature, heating rate are 10 DEG C/min, are incubated 1 hour, second step be placed on nitrogen pressure for 2.1～
8.0MPa, 1400 DEG C～1830 DEG C of temperature, heating rate are 10 DEG C/min, are incubated 1 hour.
Using defat and two-step method idiosome, can prepare and rub with fine microstructure and high performance Sialon ceramics
Wipe weldering stirring-head.
Present invention simultaneously provides using the process for preparing and matching that ceramic friction welds stirring-head, what is prepared has
The stirring-head of lightweight, high-strength and high ductility, high temperature resistant and excellent wear-resisting property.
Compared with prior art, the invention has the advantages that：
The present invention is directed to the high existing high temperature resistant stirring-head cost of raw material, complicated process of preparation, difficult processing and processing capacity
Greatly, the high problem of manufacturing cost, there is provided a kind of low cost, the process of dead size molding Sialon ceramics stirring-head, it is prepared
Stirring-head the features such as there is lightweight, high-strength and high ductility, high temperature resistant and excellent wear-resisting property.
Sialon ceramics has preferable toughness, very high hardness and wearability, and very high high-temperature oxidation resistance, and
And the Sialon ceramics prices of raw materials are cheap, wide material sources.
Low temperature injection molding dead size moulding process, its process is simple, parameter are controllable, easily prepare Complex Different Shape size stirring-head,
Semifinished product precision is high, and allowance is few, substantially reduces the preparation cost of stirring-head and its cost of through engineering approaches application；And by original
Material constituent element is designed and preparation technology parameter adjustment, easily realizes the optimization and regulation and control of the organizational structure and performance of stirring-head.
The Sialon ceramics stirring-head high temperature resistant (more than 1000 DEG C) of preparation, intensity and toughness are high, wearability is good, service life
It is long.
Description of the drawings
Fig. 1 present invention plants X-ray diffraction (XRD) figure of Sialon ceramics friction welding (FW) stirring-head.
Fig. 2 present invention plants scanning electron microscope (SEM) figure of Sialon ceramics friction welding (FW) stirring-head.
Specific embodiment
The present invention is further described with specific embodiment below in conjunction with the accompanying drawings.Unless stated otherwise, the present invention is implemented
The various raw materials that example is used can be obtained by routine is commercial, or are prepared according to the conventional method of this area, used to set
Standby is experiment common equipment.Unless otherwise defined or described herein, all specialties used herein and scientific words and this area
Same meaning familiar to person skilled in the art institute.
Embodiment 1
A kind of process for preparing Sialon ceramics friction welding (FW) stirring-head, comprises the following steps：
S1. prepare Sialon ceramics powder：According to molecular formula Si of Sialon ceramics4Al2O2N6Calculate and weigh weighing corresponding
Si3N4, AlN and Al2O3, add 3wt%Y2O3, gained batch mixing is carried out into ball milling, then 6h is dried in 80 DEG C of baking ovens, it is close
Envelope；
Wherein ball milling is further comprising the steps of：
S11. by batch mixing, different size of corundum and dehydrated alcohol according to mass ratio 1:1.5:2 load in agate jar；
S12. the ball grinder for installing sealing is put into into ball milling 20h in planetary ball mill.
S2. gel casting forming：
S21. configure premixed liquid：15wt%N- n-methylolacrylamide, 9wt%N, N- dimethyl-ethylenediamines and 5vol% gather
Ammonium acrylate, wherein ammonium polyacrylate are dissolved in deionized water, and adjust pH value for 9 with ammonia.
S22. premixed liquid obtained by step S21 is added in the Sialon ceramics powder obtained by step S1, after mixing, adds 8wt%'s
Y2O3With the Al of 5%wt%2O3Used as sintering aid, ball milling is 4h, obtains required injection molding slurry；
S23. the ammonium persulfate solution and 5wt% of 10wt% by injection molding slurry obtained by step S22 Jing after froth in vacuum, are added
Tetramethylethylenediamine, after being uniformly mixed inject polymorphic structure stirring-head mould, after normal temperature cure molding, in 50 DEG C of baking
It is dried to quality in case and no longer becomes；
S3. defat and sintering：
S31., under 0.05Mpa nitrogen atmospheres, base substrate degreasing is completed to 800 DEG C with the heating rate of 1 DEG C/min.
S32. defat idiosome in S31 being placed on into nitrogen pressure for 0.1MPa, temperature is 1150 DEG C, heating rate is 10 DEG C/
Min, is incubated 1h；
S33. it is 2.1MPa later idiosome will to be processed in S32 steps and is placed on nitrogen pressure, and temperature is 1400 DEG C, and heat up speed
Rate is 10 DEG C/min, is incubated 1h.
Embodiment 2
A kind of process for preparing Sialon ceramics friction welding (FW) stirring-head, comprises the following steps：
S1. prepare Sialon ceramics powder：According to molecular formula Si of Sialon ceramics4Al2O2N6Calculate and weigh weighing corresponding
Si3N4, AlN and Al2O3, add 6wt%Y2O3, gained batch mixing is carried out into ball milling, then 10h is dried in 80 DEG C of baking ovens, it is close
Envelope；
Wherein ball milling is further comprising the steps of：
S11. by batch mixing, different size of corundum and dehydrated alcohol according to mass ratio 1:1.5:2 load in agate jar；
S12. the ball grinder for installing sealing is put into into ball milling 24h in planetary ball mill.
S2. gel casting forming：
S21. configure premixed liquid：20wt%N- n-methylolacrylamide, 10wt%N, N- dimethyl-ethylenediamines and 6vol%
Ammonium polyacrylate, wherein ammonium polyacrylate are dissolved in deionized water, and adjust pH value for 10 with ammonia.
S22. premixed liquid obtained by step S21 is added in the Sialon ceramics powder obtained by step S1, after mixing, adds 10wt%
Y2O3With the Al of 7%wt%2O3Used as sintering aid, ball milling is 6h, obtains required injection molding slurry；
S23., injection molding slurry obtained by step S22 is added Jing after froth in vacuum the ammonium persulfate solution and 6wt% of 12wt%
Tetramethylethylenediamine, after being uniformly mixed inject polymorphic structure stirring-head mould, after normal temperature cure molding, in 80 DEG C of baking
It is dried in case, no longer becomes to quality；
S3. defat and sintering：
S31., under 0.1Mpa nitrogen atmospheres, base substrate degreasing is completed to 900 DEG C with the heating rate of 1 DEG C/min.
S32. it is 2.1MPa defat idiosome in S31 to be placed on nitrogen pressure, and temperature is 1600 DEG C, with heating rate as 10
DEG C/min, it is incubated 1h；
S33. it is 8.0MPa later idiosome will to be processed in S32 steps and is placed on nitrogen pressure, and temperature is 1600 DEG C, and heat up speed
Rate is 10 DEG C/min, is incubated 1h.
Embodiment 3
A kind of process for preparing Sialon ceramics friction welding (FW) stirring-head, comprises the following steps：
S1. prepare Sialon ceramics powder：According to molecular formula Si of Sialon ceramics4Al2O2N6Calculate and weigh weighing corresponding
Si3N4, AlN and Al2O3, add 4wt%Y2O3, gained batch mixing is carried out into ball milling, then 7h is dried in 80 DEG C of baking ovens, it is close
Envelope；
Wherein ball milling is further comprising the steps of：
S11. by batch mixing, different size of corundum and dehydrated alcohol according to mass ratio 1:1.5:2 load in agate jar；
S12. the ball grinder for installing sealing is put into into ball milling 21h in planetary ball mill.
S2. gel casting forming：
S21. configure premixed liquid：16wt%N- n-methylolacrylamide, 10wt%N, N- dimethyl-ethylenediamines and 6vol%
Ammonium polyacrylate, wherein ammonium polyacrylate are dissolved in deionized water, and adjust pH value for 9 with ammonia.
S22. premixed liquid obtained by step S21 is added in the Sialon ceramics powder obtained by step S1, after mixing, adds 9wt%'s
Y2O3With the Al of 6%wt%2O3Used as sintering aid, ball milling is 5h, obtains required injection molding slurry；
S23., injection molding slurry obtained by step S22 is added Jing after froth in vacuum the ammonium persulfate solution and 6wt% of 11wt%
Tetramethylethylenediamine, after being uniformly mixed inject polymorphic structure stirring-head mould, after normal temperature cure molding, in 60 DEG C of baking
It is dried to quality in case and no longer becomes；
S3. defat and sintering：
S31., under 0.06Mpa nitrogen atmospheres, base substrate degreasing is completed to 900 DEG C with the heating rate of 1 DEG C/min.
S32. defat idiosome in S31 being placed on into nitrogen pressure for 1.5MPa, temperature is 1850 DEG C, heating rate is 10 DEG C/
Min, is incubated 1h；
S33. it is 4MPa later idiosome will to be processed in S32 steps and is placed on nitrogen pressure, and temperature is 1830 DEG C, heating rate
For 10 DEG C/min, 1h is incubated.
Microstructure and performance characterization are carried out to arbitrarily gained Sialon pottery friction welding (FW) stirring-head in 1～embodiment of embodiment 3
It is as follows with test result:
1. prepared Sialon ceramics is stirred using the 2550 type XRD diffractometers of D/max of Rigaku Electric Co., Ltd
Mixing head material carries out material phase analysis, and its XRD is as shown in Figure 1.As shown in Figure 1, the thing phase composition of prepared stirring-head is main
For α-Sai Long and β-Sai Long.
2. using the JSM-6360LV types electronic scanner microscope of Jeol Ltd. to prepared stirring-head
Microstructure is analyzed, and its result is as shown in Figure 2.As shown in Figure 2, all α-Sai Long crystal grain in sample top layer, in thick
Column crystal must, and in internal layer, there are elongated crystal whisker-shaped β-Sai Long crystal grain, α-Sai Long crystal grain also has in crystal whisker-shaped, but compares
Top layer it is tiny.
The performance test results and sign:
Gained stirring-head is prepared to 1～embodiment of embodiment 3 carries out performance detection, specifically：Surveyed using Archimedes method
The density of amount material, each data are at least surveyed three samples and are averaged.Produced using Laizhou Huayi Testing Instrument Co., Ltd.
HV-10A Vickers, determine Vickers hardness, load 1kg, load 10s, test five points, average.Sample it is anti-
Bending strength test process reference《Engineering ceramics bending strength test method》(GB6569-86) carry out, in CSS-44100 electronics
Determined using three-point bending method on universal testing machine.When bending strength is tested, specimen size is 4mm × 3mm × 36mm (width x thickness
× long), span 30mm, loading speed are 0.5mm/min.Sample tension mirror polish, and require chamfering (45 °).Using
Vicker indentation methods measure the fracture toughness of material, the HV-10A Vickers that impression is produced by Laizhou Huayi Testing Instrument Co., Ltd.
Durometer is produced, and loading speed is 0.5mm/min, load 10kg, load time 10s.Concrete testing result is as shown in table 1.
1 stirring-head main performance index of table
| Embodiment | Density (g/cm3) | Vickers hardness (HV) | Bending strength (Mpa) | Fracture toughness (MPa m1/2) |
| Embodiment 1 | 3.210 | 1538 | 736 | 7.268 |
| Embodiment 2 | 3.206 | 1546 | 763 | 7.198 |
| Embodiment 3 | 3.205 | 1525 | 714 | 7.464 |
Claims (10)
1. a kind of process for preparing Sialon ceramics friction welding (FW) stirring-head, it is characterised in that comprise the following steps：
S1. prepare Sialon ceramics powder：According to molecular formula Si of Sialon ceramics4Al2O2N6Calculate and weigh the corresponding Si of weighing3N4、
AlN and Al2O3, add Y2O3After obtain batch mixing, gained batch mixing is carried out into ball milling, then dried, seal；
S2. gel casting forming：
S21. premixed liquid is configured, the premixed liquid includes N hydroxymethyl acrylamide, N, N- dimethyl-ethylenediamines and polyacrylic acid
Ammonium；
S22. step S21 premixed liquid is added in the Sialon ceramics powder obtained by step S1, carries out ball milling, obtain required injection molding slurry
Material；
S23., by injection molding slurry obtained by step S22 Jing after froth in vacuum, ammonium persulfate solution and tetramethylethylenediamine, stirring are added
Polymorphic structure stirring-head mould is injected after mix homogeneously, after normal temperature cure molding, process is dried；
S3. defat and sintering：S2 prepared base substrate is put into nitrogen atmosphere stove carries out temperature programming, first completes defat, then adopts
Two-step method molding, obtains the Sialon ceramics friction welding (FW) stirring-head.
2. the process of Sialon ceramics friction welding (FW) stirring-head is prepared according to claim 1, it is characterised in that step S1 institute
It is, in 80 DEG C of baking ovens, to be dried 6～10h to state dried.
3. the process of Sialon ceramics friction welding (FW) stirring-head is prepared according to claim 1, it is characterised in that step S1 institute
State Y2O3For 3～6wt%.
4. the process of Sialon ceramics friction welding (FW) stirring-head is prepared according to claim 1, it is characterised in that step S1 institute
State ball milling further comprising the steps of：
S11. by batch mixing, mill ball and ball-milling medium according to mass ratio 1:1.5:2 load in ball grinder；The mill ball is not from
With the corundum of size, the ball-milling medium selects dehydrated alcohol, the ball grinder to select agate jar；
S12. the ball grinder for installing sealing is put into into 20～24h of ball milling in planetary ball mill.
5. the process of Sialon ceramics friction welding (FW) stirring-head is prepared according to claim 1, it is characterised in that step S21
The N hydroxymethyl acrylamide be 15～20wt%, the N, N- dimethyl-ethylenediamines be 9～10wt%, the ammonium polyacrylate
For 5～6vol%, it is preferable that the ammonium polyacrylate is dissolved in deionized water, and pH value is adjusted for 9～10 with ammonia.
6. the process of Sialon ceramics friction welding (FW) stirring-head is prepared according to claim 1, it is characterised in that step S22
The ball milling adds the Y of 8～10wt% in being additionally included in mixed liquor2O3With the Al of 5～7wt%2O3As sintering aid, during ball milling
Between be 4～6h.
7. the process of Sialon ceramics friction welding (FW) stirring-head is prepared according to claim 1, it is characterised in that step S23
The ammonium persulfate solution is 10～12wt%, and the tetramethylethylenediamine is 5～6wt%.
8. the process of Sialon ceramics friction welding (FW) stirring-head is prepared according to claim 1, it is characterised in that step S23
The dried is, in 50～80 DEG C of baking oven, to be dried to quality and no longer change.
9. the process of Sialon ceramics friction welding (FW) stirring-head is prepared according to claim 1, it is characterised in that step S3 institute
State defat to refer under 0.05～0.1Mpa nitrogen atmospheres, defat is completed to 800～900 DEG C with the heating rate of 1 DEG C/min；Institute
State two-step method and refer to that green compact are placed on nitrogen pressure for 0.1～2.1MPa, 1150 DEG C～1850 DEG C of temperature, intensification by the first step
Speed is 10 DEG C/min, is incubated 1 hour, and second step is placed on nitrogen pressure for 2.1～8.0MPa, 1400 DEG C～1830 DEG C of temperature,
Heating rate is 10 DEG C/min, is incubated 1 hour.
10. the Sialon ceramics friction welding (FW) stirring-head that the process according to claim 1 to 9 any one is prepared.
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| CN107962293A (en) * | 2017-12-14 | 2018-04-27 | 湘潭大学 | The integrated molding method of materials with high melting point stirring friction welding agitator head |
| CN109734457A (en) * | 2019-01-24 | 2019-05-10 | 湖南工业大学 | A kind of high rigidity Sialon ceramic material and its preparation method and application |
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