CN102430757A - Method for preparing TiB2/TiC (titanium diboride/titanium carbide) ultrafine powder for surface spraying of engine piston ring by means of high energy ball milling - Google Patents
Method for preparing TiB2/TiC (titanium diboride/titanium carbide) ultrafine powder for surface spraying of engine piston ring by means of high energy ball milling Download PDFInfo
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- CN102430757A CN102430757A CN2011103816234A CN201110381623A CN102430757A CN 102430757 A CN102430757 A CN 102430757A CN 2011103816234 A CN2011103816234 A CN 2011103816234A CN 201110381623 A CN201110381623 A CN 201110381623A CN 102430757 A CN102430757 A CN 102430757A
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Abstract
The invention discloses a method for preparing TiB2/TiC (titanium diboride/titanium carbide) ultrafine powder for surface spraying of an engine piston ring by means of high energy ball milling. The method includes the steps: (1) weighing Ti (titanium) powder and B4C (boron carbide) powder as powder materials, (2) weighing grinding balls, (3) placing the powder materials into a ball milling tank and then covering the powder materials with the grinding balls so as to press the upper surfaces of all the powder materials, (4) leading inert gas into the ball milling tank so as to exhaust air, and (5) performing ball milling. The method for mechanical alloying by means of high energy ball milling is used for in-situ synthesis of nanoscale metal ceramic composite TiB2/TiC powder, vacuum pumping and argon filling during in-situ synthesis do not need to be performed in a vacuum glove box, accordingly, operation procedures are simplified, production efficiency is improved, and the method is suitable for industrial production.
Description
Technical field
The invention belongs to metal material field, relate to a kind of prepared by mechanical alloy nanoscale TiB that utilizes
2The method at/TiC metal-ceramic composite powder end.
Background technology
TiB
2With TiC as cermet material, have all that fusing point height, steam force down, advantages such as electric conductivity is good, hardness is high, excelling in abrasion resistance.TiB
2Regarded as one of promising material by widely research with TiC because of having above-mentioned a series of good performance.At present, TiB
2Be widely used in as particulate reinforced composite, composite ceramic material, hard alloy substrate, cathodic protection material, conducting ceramic material in industries such as metallurgy, machinery, military affairs, chemical industry, electronics with TiC, the various countries researchers have been placed on focus and nanoscale TiB in recent years
2In the research and development of the various new materials relevant with TiC.Preparation TiB
2Method mainly contain direct synthesis technique, self propagating high temperature synthetic method (metallothermic processes), nonmetal thermal reduction (carbothermic method), boron carbide method, fused salt electrolysis process, chemical meteorology deposition method, plasma-arc oven process etc.And synthetic solid-state synthetic method, carbon reduction method, bath of molten metal synthetic method, gas-phase reaction synthetic method, the shock wave method etc. of mainly containing of TiC.In the spraying of HVAF technology (HVOF) engine piston ring surface, experience learns that the figure layer that the used powder of spraying more carefully obtains is not easy to be stripped from more, therefore uses superfine powder can significantly improve the whole anti-wear performance of figure layer.And at present, commercially available TiB
2Powder mainly be particle diameter more than 2 microns, adopt carbon reduction method and metallothermic processes to be prepared from.Also can prepare nanoscale TiB as self propagating high temperature is synthetic
2, but need processing such as following process pickling, fragmentation, not desirable method obviously.Therefore can prepare pure nano level TiB simultaneously
2With TiC metal-ceramic composite powder end and can be applied to commercial production then be that researchers expect.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of method that adopts high-energy ball milling machinery alloying is provided, original position synthesis nano metal-ceramic composite powder end TiB
2/ TiC; The applying argon gas that vacuumizes of this process need not in vacuum glove box, to operate, thereby the flow process that simplifies the operation, enhances productivity, and is adapted at using in the commercial production.
The object of the invention is achieved through following technical proposals:
A kind of high-energy ball milling prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder, carry out according to following step:
(1) takes by weighing Ti powder and B
4The C powder is as powder, wherein Ti and B
4The mol ratio of C is 3: 1, dries then, and drying time is 12～24 hours, and bake out temperature is 60～150 ℃; Preferred drying time is 15～20 hours, and bake out temperature is 60～100 ℃;
(2) weighing abrading-ball, wherein the mass ratio of powder is (2: 1)-(20: 1) in abrading-ball and the step (1); The mass ratio of preferred abrading-ball and powder is (2: 1)-(10: 1);
(3) with powder as in the ball grinder; Cover so that the upper surface of all powders is all pushed down by abrading-ball with abrading-ball then; Wherein abrading-ball and powder account for 1/2～2/3 of ball grinder volume; Preferably that diameter is minimum abrading-ball is close to powder, and the ball that diameter is bigger is being pressed less ball, makes all powders except that intermediate gaps, all pushed down by abrading-ball;
(4) in ball grinder, feed inert gas, inert gas flow velocity air pressure is 0-0.1Mpa; Preferably the tube head of gas is deep in the ball grinder abrading-ball top and ventilates, adopt argon gas; Because the molal weight (40) of argon gas is higher than the average molar mass (29) of air, so argon gas can sink to the below of air, to discharge air;
(5) the sealing ball grinder carries out ball milling, and drum's speed of rotation is 50-530r/min, and the ball milling time is 5-60 hour, and ball grinding method is dry grinding; The preferred spheres mill speed is 300-530r/min, and the ball milling time is 20-50 hour.
In the technical scheme of the present invention, when the conducting powder material extracts after the ball-milling reaction, if powder is bonded on ball milling tank skin or the abrading-ball, then add a small amount of alcohol, continuing wet-milling 30 seconds-2 minutes, 60-150 ℃ of oven dry taken out the nature cooling until whole dryings then.
The present invention compares the advantage that is had with prior art and is: reaction raw materials is cheap, need not extra heat source, product is pure (has only TiB
2With TiC two mutually), need not subsequent treatment (like pickling etc.); Simplified the process that vacuumizes applying argon gas; Make easy and simple to handlely, productivity ratio improves, and is fit to large-scale commercial production more; Though but the argon gas that charges into is unlike in the such high-purity production effect that do not influence that carries out in the vacuum glove box, pure contains TiB in the product
2With TiC two mutually, and the TiC particle diameter can reach 5-12 nanometer, TiB
2Particle diameter can reach the 80-600 nanometer, is perfect condition, TiB
2All have higher hardness and wearability with TiC itself.
Description of drawings
The TEM photo (the TEM model is JEOL, and manufacturer is a NEC) of the inorganic powder of Fig. 1 the present invention preparation.
The XRD figure of the inorganic powder of Fig. 2 the present invention preparation (the XRD model is the XRD7000 type, and manufacturer is day island proper Tianjin).
The specific embodiment
Further specify technical scheme of the present invention below in conjunction with the specific embodiment.The model of selecting for use Nanjing Univ. Instrument Factory to produce is that the planetary ball mill of QM-3SP4J prepares.
Embodiment 1
1. with Ti and B
4C amounts to 50g according to 3: 1 molar ratio weighing, and 80 ℃ of oven dry 20 hours are for use;
2. by 10: 1 weighing diameters 6,10,12 of ratio of grinding media to material, 20mm stainless steel ball, amount to 500g, for use;
3. select the stainless steel jar mill of 250Ml for use, at first reactant is put into stainless cylinder of steel, on powder, put into ball then; Almost except some slits, can cover powder fully, the ball material accounts for 2/3 of ball grinder volume altogether; Afterwards the argon gas tube head deeply is deep into the position of one deck ball topmost along the ball grinder inwall; Argon gas flow velocity air pressure is 0.1Mpa, takes away the sealing ball grinder after 10 minutes;
4. selecting rotating speed is 300r/min, and ball milling 60 hours, machine are set at ball milling rest half an hour half an hour;
5. after 60 hours, open ball grinder and add a small amount of alcohol (flooding ball gets final product), sealing ball milling 2 minutes, it is dry to take out back low temperature drying to powder.
Embodiment 2
1. with Ti and B
4C amounts to 50g according to 3: 1 molar ratio weighing, and 80 ℃ of oven dry 20 hours are for use;
2. by 10: 1 weighing diameters 6,8,12 of ratio of grinding media to material, 20mm stainless steel ball, amount to 500g, for use;
3. select the stainless steel jar mill of 250Ml for use, at first reactant is put into stainless cylinder of steel, on powder, put into ball then; Almost except some slits, can cover powder fully, the ball material accounts for 2/3 of ball grinder volume altogether; Afterwards the argon gas tube head deeply is deep into the position of one deck ball topmost along the ball grinder inwall; Argon gas flow velocity air pressure is 0.1Mpa, takes away the sealing ball grinder after 10 minutes;
4. selecting rotating speed is 400r/min, and ball milling 40 hours, machine are set at ball milling rest half an hour half an hour;
5. after 40 hours, open ball grinder and add a small amount of alcohol (flooding ball gets final product), sealing ball milling 2 minutes, it is dry to take out back low temperature drying to powder.
Embodiment 3
1. with Ti and B
4C amounts to 50g according to 3: 1 molar ratio weighing, and 80 ℃ of oven dry 20 hours are for use;
2. by 15: 1 weighing diameters 6,8,10 of ratio of grinding media to material, 20mm stainless steel ball, amount to 750g, for use;
3. select the stainless steel jar mill of 250Ml for use, at first reactant is put into stainless cylinder of steel, on powder, put into ball then; Almost except some slits, can cover powder fully, the ball material accounts for 2/3 of ball grinder volume altogether; Afterwards the argon gas tube head deeply is deep into the position of one deck ball topmost along the ball grinder inwall; Argon gas flow velocity air pressure is 0.1Mpa, takes away the sealing ball grinder after 10 minutes;
4. selecting rotating speed is 500r/min, and ball milling 20 hours, machine are set at ball milling rest half an hour half an hour;
5. after 20 hours, open ball grinder and add a small amount of alcohol (flooding ball gets final product), sealing ball milling 2 minutes, it is dry to take out back low temperature drying to powder.
Embodiment 4
1. with Ti and B
4C amounts to 50g according to 3: 1 molar ratio weighing, and 80 ℃ of oven dry 20 hours are for use;
2. by 15: 1 weighing diameters 8,10,12 of ratio of grinding media to material, 20mm stainless steel ball, amount to 750g, for use;
3. select the stainless steel jar mill of 250Ml for use, at first reactant is put into stainless cylinder of steel, on powder, put into ball then; Almost except some slits, can cover powder fully, the ball material accounts for 2/3 of ball grinder volume altogether; Afterwards the argon gas tube head deeply is deep into the position of one deck ball topmost along the ball grinder inwall; Argon gas flow velocity air pressure is 0.1Mpa, takes away the sealing ball grinder after 10 minutes;
4. selecting rotating speed is 400r/min, and ball milling 10 hours, machine are set at ball milling rest half an hour half an hour;
5. after 10 hours, open ball grinder and add a small amount of alcohol (flooding ball gets final product), sealing ball milling 2 minutes, it is dry to take out back low temperature drying to powder.
Embodiment 5
1. with Ti and B
4C amounts to 50g according to 3: 1 molar ratio weighing, and 80 ℃ of oven dry 20 hours are for use;
2. by 20: 1 weighing diameters 6,8,10 of ratio of grinding media to material, 12mm stainless steel ball, amount to 1000g, for use;
3. select the stainless steel jar mill of 250Ml for use, at first reactant is put into stainless cylinder of steel, on powder, put into ball then; Almost except some slits, can cover powder fully, the ball material accounts for 2/3 of ball grinder volume altogether; Afterwards the argon gas tube head deeply is deep into the position of one deck ball topmost along the ball grinder inwall; Argon gas flow velocity air pressure is 0.1Mpa, takes away the sealing ball grinder after 10 minutes;
4. selecting rotating speed is 400r/min, and ball milling 50 hours, machine are set at ball milling rest half an hour half an hour;
5. after 50 hours, open ball grinder and add a small amount of alcohol (flooding ball gets final product), sealing ball milling 2 minutes, it is dry to take out back low temperature drying to powder.
Embodiment 6
1. with Ti and B
4C amounts to 50g according to 3: 1 molar ratio weighing, and 80 ℃ of oven dry 20 hours are for use;
2. by 15: 1 weighing diameters 8,10,12 of ratio of grinding media to material, 20mm stainless steel ball, amount to 1000g, for use;
3. select the stainless steel jar mill of 250Ml for use, at first reactant is put into stainless cylinder of steel, on powder, put into ball then; Almost except some slits, can cover powder fully, the ball material accounts for 2/3 of ball grinder volume altogether; Afterwards the argon gas tube head deeply is deep into the position of one deck ball topmost along the ball grinder inwall; Argon gas flow velocity air pressure is 0.1Mpa, takes away the sealing ball grinder after 10 minutes;
4. selecting rotating speed is 500r/min, and ball milling 30 hours, machine are set at ball milling rest half an hour half an hour;
5. after 30 hours, open ball grinder and add a small amount of alcohol (flooding ball gets final product), sealing ball milling 2 minutes, it is dry to take out back low temperature drying to powder.
Embodiment 7
1. with Ti and B
4C is according to 3: 1 molar ratio weighing 100g, and 80 ℃ of oven dry 20 hours are for use;
2. by 2: 1 weighing diameters 2,5,6 of ratio of grinding media to material, 8mm zirconia ball 200g, for use;
3. select zirconia ball milling jar and the abrading-ball of 150Ml for use, at first reactant is put into jar, on powder, put into ball then; Can cover powder fully; The ball material accounts for 1/2 of ball grinder cumulative volume, afterwards the argon gas tube head deeply is deep into the position of one deck ball topmost along the ball grinder inwall, and argon gas flow velocity air pressure is 0.1Mpa; Take away the sealing ball grinder after 10 minutes;
4. select drum's speed of rotation 300r/min, ball milling 20 hours, machine are set at every ball milling and had a rest 10 minutes half an hour;
5. after 20 hours, open ball grinder and add a small amount of alcohol (flooding ball gets final product), sealing ball milling 1 minute, take out back low temperature drying to powder drying and gets final product.
Embodiment 8
1. with Ti and B
4C is according to 3: 1 molar ratio weighing 100g, and 80 ℃ of oven dry 20 hours are for use;
2. by 4: 1 weighing diameters 2,5,6 of ratio of grinding media to material, 8mm zirconia ball 400g, for use;
3. select zirconia ball milling jar and the abrading-ball of 150Ml for use, at first reactant is put into jar, on powder, put into ball then; Can cover powder fully; The ball material accounts for 2/3 of ball grinder cumulative volume, afterwards the argon gas tube head deeply is deep into the position of one deck ball topmost along the ball grinder inwall, and argon gas flow velocity air pressure is 0.1Mpa; Take away the sealing ball grinder after 10 minutes;
4. select drum's speed of rotation 500r/min, ball milling 10 hours, machine are set at every ball milling and had a rest 10 minutes half an hour;
5. after 10 hours, open ball grinder and add a small amount of alcohol (flooding ball gets final product), sealing ball milling 1 minute, take out back low temperature drying to powder drying and gets final product.
More than the present invention has been done exemplary description; Should be noted that; Under the situation that does not break away from core of the present invention, the replacement that is equal to that any simple distortion, modification or other those skilled in the art can not spend creative work all falls into protection scope of the present invention.
Claims (9)
1. a high-energy ball milling prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder is characterized in that, carries out according to following step:
(1) takes by weighing Ti powder and B
4The C powder is as powder, wherein Ti and B
4The mol ratio of C is 3: 1, dries then;
(2) weighing abrading-ball, wherein the mass ratio of powder is (2: 1)-(20: 1) in abrading-ball and the step (1);
(3) with powder as in the ball grinder, cover so that the upper surface of all powders is all pushed down by abrading-ball with abrading-ball above then;
(4) in ball grinder, feed inert gas, to discharge air;
(5) the sealing ball grinder carries out ball milling.
2. a kind of high-energy ball milling according to claim 1 prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder is characterized in that, drying time is 12-24 hour in the said step (1), and bake out temperature is 60-150 ℃.
3. a kind of high-energy ball milling according to claim 2 prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder is characterized in that, drying time is 15-20 hour in the said step (1), and bake out temperature is 60-100 ℃.
4. a kind of high-energy ball milling according to claim 1 prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder is characterized in that, the mass ratio of abrading-ball and powder is (2: 1)-(10: 1) in the said step (2).
5. a kind of high-energy ball milling according to claim 1 prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder; It is characterized in that abrading-ball and powder account for the 1/2-2/3 of ball grinder volume in the said step (3), preferably that diameter is minimum abrading-ball is close to powder; The ball that diameter is bigger is being pressed less ball, makes all powders except that intermediate gaps, all pushed down by abrading-ball.
6. a kind of high-energy ball milling according to claim 1 prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder is characterized in that, inert gas flow velocity air pressure is 0-0.1Mpa in the said step (4).
7. a kind of high-energy ball milling according to claim 6 prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder is characterized in that, preferred tube head with gas is deep in the ball grinder and ventilates above the abrading-ball in the said step (4), and the employing argon gas is an inert gas.
8. a kind of high-energy ball milling according to claim 1 prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder is characterized in that, drum's speed of rotation is 400-1000r/min in the said step (5), and the ball milling time is 5-60 hour, and ball grinding method is dry grinding.
9. a kind of high-energy ball milling according to claim 8 prepares the spraying of engine piston ring surface and uses TiB
2The method of/TiC superfine powder is characterized in that, the preferred spheres mill speed is 600-1000r/min in the said step (5), and the ball milling time is 20-50 hour.
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Cited By (4)
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| CN107020372A (en) * | 2017-04-26 | 2017-08-08 | 武汉理工大学 | A kind of water-based spray prilling process of titanium diboride/nickel molybdenum composite granule |
| CN108018442A (en) * | 2017-06-12 | 2018-05-11 | 吉林大学 | It is micro-nano to mix TiC-TiB2Particle strengthening high-performance aluminium alloy preparation method |
| CN110592426A (en) * | 2019-08-27 | 2019-12-20 | 江苏大学 | High-hardness high-temperature-resistant TiC + TiB reinforced titanium-based composite material generated by solid-phase in-situ reaction and preparation method thereof |
| CN115070038A (en) * | 2022-07-21 | 2022-09-20 | 西安稀有金属材料研究院有限公司 | In-situ mixed dual-phase ceramic reinforced iron-based composite material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107020372A (en) * | 2017-04-26 | 2017-08-08 | 武汉理工大学 | A kind of water-based spray prilling process of titanium diboride/nickel molybdenum composite granule |
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| CN108018442A (en) * | 2017-06-12 | 2018-05-11 | 吉林大学 | It is micro-nano to mix TiC-TiB2Particle strengthening high-performance aluminium alloy preparation method |
| CN110592426A (en) * | 2019-08-27 | 2019-12-20 | 江苏大学 | High-hardness high-temperature-resistant TiC + TiB reinforced titanium-based composite material generated by solid-phase in-situ reaction and preparation method thereof |
| CN110592426B (en) * | 2019-08-27 | 2021-11-23 | 江苏大学 | High-hardness high-temperature-resistant TiC + TiB reinforced titanium-based composite material generated by solid-phase in-situ reaction and preparation method thereof |
| CN115070038A (en) * | 2022-07-21 | 2022-09-20 | 西安稀有金属材料研究院有限公司 | In-situ mixed dual-phase ceramic reinforced iron-based composite material and preparation method thereof |
| CN115070038B (en) * | 2022-07-21 | 2022-11-04 | 西安稀有金属材料研究院有限公司 | In-situ mixed dual-phase ceramic reinforced iron-based composite material and preparation method thereof |
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Application publication date: 20120502 |