CN105734318A - Method for preparing nano-gradient composite W-Cu material - Google Patents
Method for preparing nano-gradient composite W-Cu material Download PDFInfo
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- CN105734318A CN105734318A CN201610249898.5A CN201610249898A CN105734318A CN 105734318 A CN105734318 A CN 105734318A CN 201610249898 A CN201610249898 A CN 201610249898A CN 105734318 A CN105734318 A CN 105734318A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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Abstract
The invention relates to the field of nano materials and powder metallurgy, in particular to a method for preparing a nano-gradient composite W-Cu material. W-Cu composite powder containing various components is prepared; by controlling the granularity and morphology of the composite powder, the sintering activity of the W-Cu composite powder containing the different components is changed, and therefore the W-Cu composite powder which contains the different components and can be sintered to be approximately fully dense at the same temperature is obtained; the nano composite W-Cu powder is subjected to layering and powder spreading in sequence from the high copper content to the low copper content and then to pressing forming; and the nano-gradient composite W-Cu material is obtained after demolding, presintering and one-step liquid phase sintering. According to the method, by means of technology control over the preparation process of the composite powder, the control over the granularity, morphology and sintering densification behavior of the W-Cu composite powder is achieved, and moreover one-step sintering preparation of the multi-layer gradient composite material is achieved; the prepared W-Cu gradient composite material is high in density, fine and uniform in structure and good in interlayer bonding, and the components and properties are continuously changed in the thickness direction; and the range of the components is large, and the change range of the properties is large.
Description
Technical field
The present invention relates to nano material and field of powder metallurgy, particularly nanometer gradient and be combined the system of W-Cu material
Preparation Method.
Background technology
W-Cu gradient composites is homogenizing W-Cu composite and the product of functionally gradientization combination, has concurrently
Constituent element W, Cu and the characteristic of structure property gradient distribution.W as the highest metal of fusing point, have high intensity,
The advantage such as low thermal coefficient of expansion, Heat stability is good；Cu has good processability, high heat conduction/electrical, stablizes
The advantage such as chemical property, therefore, W-Cu gradient composites is in fields such as electronics, traffic, Aero-Space
On there is the biggest using value.
The preparation method of W-Cu gradient composites mainly has infiltration method, powder metallurgic method, plasma spray at present
Coating etc..Infiltration method is that common a kind of technique prepared by homogenizing W-Cu material, first passes through high temperature sintering added with making
Hole agent and the W base sample of induction copper, then penetrate into copper liquid in having in the W skeleton of certain porosity of preparation, its
Feature be the mechanical property of the W-Cu material prepared and electric conductivity preferable, but W skeleton sintering temperature is high,
Distribution of pores is difficult to control to, W coarse grains, uneven microstructure, and the high Cu content more difficult system of W skeleton
Standby, especially in the preparation of W-Cu gradient composites, component distributing and shape are difficult to accurately control (to receive
Contract inconsistent).Additionally, use, infiltration method is follow-up when preparing W-Cu gradient composites also to be gone with machining
Except unnecessary copper, add production cost, reduce yield rate and work efficiency.Powder metallurgic method is by difference
The W-Cu mixed powder of composition, pavement layer by layer, it is pressed into the pressed compact with gradient-structure, then passes through high-temperature liquid-phase
Sintering obtains the W-Cu composite with gradient-structure.W-Cu powder sintering temperatures due to heterogeneity
Inconsistent, there will be sample consistency at the same temperature during liquid-phase sintering the highest, and organize the phenomenons such as thick,
And then make material property poor.The plasma spraying method of W-Cu FGM is broadly divided into atmosphere plasma
Spraying (APS) and vacuum (low pressure) plasma spraying (VPS), this method is by controlling technological parameter (spray
The component ratio of powder, temperature and spraying rate etc.) adjust coating structure and composition.But, this method system
Owing to the combination between each layer is based on mechanical bond in standby W-Cu gradient composites, bond strength is low,
And functionally gradient material (FGM) porosity is high, the binding site of each gradient layer easily peels off.
Recent study shows, by improving W-Cu composite powder homogeneity of ingredients and reducing powder size and can show
Write the intermiscibility alleviating W and Cu, and then improve liquid-phase sintering densification.The research of this respect mainly has height
Can ball-milling technology and thermochemical processes.Traditional high-energy-milling, can reduce powder size, increase Cu
Solid solubility in W, obtains the single component W-Cu composite of high-compactness.Inventor herein exists
Last stage has applied for and has obtained a national inventing patent " preparation method of thin brilliant tungsten-copper composite material " (patent
Number: ZL200510031446.1), this patent, with solubility tungsten salt, mantoquita crystal as raw material, uses colloidal sol spray
Mist is dried-ultra-fine/W-Cu nanocomposite powder of preparing of calcining reduction technique, and powder purity is high, densified sintering product
Change temperature more conventional W-Cu powder substantially to reduce, available high brilliant W-Cu fine and close, thin after low temperature one step sintering
Composite.But W-Cu composite prepared by these methods causes different Cu content due to composition difference
W-Cu composite powder needs different sintering temperatures to be issued to full densification, and this allows for using nano combined W-Cu
When powder directly prepares functionally gradient material (FGM) process there is difficult point in the selection of sintering gradient material temperature, is extremely difficult to one
The closely full consistency sintering of functionally gradient material (FGM) is realized at individual temperature.
Summary of the invention
Exist in terms of material property and densification for the gradient W-Cu composite prepared by above method
Problem, the present invention combines existing achievement in research, uses nanometer composite technology to prepare ultra-fine/nanograined W-Cu multiple
Close powder, changed the W-Cu composite powder of heterogeneity by the control granularity of W-Cu composite powder, pattern
The sintering activity at end, it is achieved the W-Cu composite powder of heterogeneity sinters near complete fine and close at the same temperature, enters
And use the compacting of place Min layers powder and a step sintering to prepare crystal grain full densification tiny, uniform, near and gradient layer each layer knot
Close intact W-Cu gradient composites.Nanometer gradient prepared by the present invention is combined the consistency of W-Cu material
Up to more than 98.5%, alloy structure fine uniform, Coating combination performance is good, and material property through-thickness is even
Continuous change.
The present invention is for reaching above-mentioned purpose, and the concrete scheme of employing is as follows:
(1) use in colloidal sol-spray drying-thermal reduction technology, Mechanic Alloying Technology, sol-gel technique
One or more prepare the W-Cu composite powder of Multiple components, by control final composite powder granularity,
Pattern, and then change the sintering activity of the W-Cu composite powder of heterogeneity, it is thus achieved that can burn at the same temperature
Tie the W-Cu composite powder of nearly fully dense heterogeneity；
Concrete, colloidal sol-spray drying-thermal reduction preparation has the nano combined of same densification temperature
W-Cu powder: copper content controls at 400-500 DEG C in the W-Cu composite powder calcining heat of 10-30wt.%,
Reduction temperature controls at 600-750 DEG C, and the recovery time is at 1-2h；Copper content is multiple at the W-Cu of 30-40wt.%
Closing powder calcining heat and control at 500-700 DEG C, reduction temperature controls at 750-850 DEG C, and the recovery time is at 2-3h；
Copper content controls at 700-800 DEG C in the W-Cu composite powder calcining heat of 40-60wt.%, reduction temperature control
System is at 800-900 DEG C, and the recovery time is at 3-4h.
Mechanical alloying preparation has the nano combined W-Cu powder of same densification temperature: copper content exists
The W-Cu composite powder ratio of grinding media to material of 10-30wt.% is 10-20:1, and rotating speed is 400-500r/min, Ball-milling Time
For 40-60 hour；Copper content is 5-15:1 in the W-Cu composite powder ratio of grinding media to material of 30-40wt.%, and rotating speed is
300-400r/min, Ball-milling Time is 20-40 hour；Copper content is at the W-Cu composite powder ball of 40-60wt.%
Material ratio is 5-10:1, and rotating speed is 300-350r/min, and Ball-milling Time is 10-20 hour；Various composite powders exist
Using argon in mechanical milling process is that protective gas prevents Powder Oxidation, carries out wet grinding with dehydrated alcohol for solvent.
Sol-gel process preparation has the nano combined W-Cu powder of same densification temperature: copper content exists
In the W-Cu composite powder solution of 10-30wt.%, solute ratio exists in 10-20wt%, calcining heat
300-400 DEG C, reduction temperature is at 500-600 DEG C, and the recovery time is at 1-2h；Copper content is 30-40wt.%'s
In W-Cu composite powder solution, solute ratio is at 20-30wt%, calcining heat at 400-500 DEG C, reduction temperature
At 600-700 DEG C, the recovery time is at 2-3h；Copper content is in the W-Cu composite powder solution of 40-60wt.%
Solute ratio is at 30-40wt%, and calcining heat is at 500-600 DEG C, and reduction temperature is at 700-800 DEG C, during reduction
Between at 3-4h.
(2) after nano combined W-Cu powder is pressed copper content place Min layers powder the most successively compressing；
Forming pressure 100～400MPa, pressurize 5-10s, the demoulding.
(3) by step (2) gained pressed compact 500～1000 DEG C of pre-burning 0.5-3h in hydrogen atmosphere, obtain many
Layer gradient W-Cu presintered compact.
(4) by step (3) gained presintered compact at 1300～1450 DEG C of one step liquid-phase sintering 0.5-3h, received
Rice graded composite W-Cu material.
The nanometer gradient that the present invention provides is combined the preparation method of W-Cu material, by preparing composite powder
The technology controlling and process of journey, reaches W-Cu composite powder granularity, pattern and the control of sintering densification behavior, enters
And realize a step sintering and prepare multi-gradient composite, the W-Cu gradient composites consistency of preparation is high,
Fine microstructures and uniformly, Coating combination is intact, and composition and performance through-thickness are consecutive variations；Composition range
Greatly, performance excursion is big, can meet the needs of various application occasions；The method sintering temperature is low, technique is simple
Singly, it is suitable for industrialized mass production.
Detailed description of the invention
It is described in conjunction with the embodiments the detailed description of the invention of the present invention.
Embodiment 1
(1) use colloidal sol-spray drying-multistep hydrogen reduction technology prepare W-10wt.%Cu, W-20wt.%Cu,
W-30wt.%Cu ultra-fine W-Cu composite powder；
(2) W-10wt.%Cu, W-20wt.%Cu, W-30wt.%Cu powder is respectively put into high-energy ball milling
In Tong, add abrading-ball by ratio of grinding media to material 10:1, add protected alcohol, be filled with argon starvation, seal ball milling,
Rotating speed 400r/min, successively ball milling 60h, 50h, 40h；
(3) vacuum drying oven is dried, collects activation W-10Cu, W-20Cu, W-30Cu composite powder,
Seal and preserve；
(4) take every kind of powder equivalent, spread powder, forming pressure 300MPa, compacting, pressurize 5s successively；
(5) pressed compact is put into pre-burning stove, be warming up to 600 DEG C with 8 DEG C/min programming rate, be incubated 30min
Pre-burning；
(6) presintered compact is sintered 90min 1380 DEG C of one step, prepare three layers of gradient W-Cu functionally gradient material
Material.
Embodiment 2
(1) use Mechanic Alloying Technology to prepare the ultra-fine W-Cu of W-15wt.%Cu, W-25wt.%Cu to be combined
Powder: W powder and Cu powder are respectively put in high-energy ball milling cylinder by W-15Cu, W-25Cu powder proportions,
Add abrading-ball by ratio of grinding media to material 20:1, add protected alcohol, be filled with argon starvation, seal ball milling, rotating speed
450r/min, successively ball milling 50h, 40h；
(3) vacuum drying oven is dried, collects activation W-15Cu, W-25Cu composite powder, seal and preserve；
(4) take every kind of powder equivalent, spread powder, forming pressure 400MPa, compacting, pressurize 5s successively；
(5) pressed compact is put into pre-burning stove, be warming up to 1000 DEG C with 10 DEG C/min programming rate, pre-burning 120min；
(6) presintered compact is sintered 120min 1450 DEG C of one step, prepare two layers of gradient W-Cu functionally gradient material
Material.
Claims (5)
1. nanometer gradient is combined the preparation method of W-Cu material, it is characterised in that include procedure below:
(1) first it is designed with nano combined W-Cu powder to prepare there is two layers, three layers or multiple structure
W-60Cu/W-10Cu gradient composites；
(2) nano combined W-Cu powder is prepared, by controlling nano combined W-Cu in powder preparing processes
The pattern of powder, granularity change the sintering activity of heterogeneity W-Cu composite powder, and then realize difference one-tenth
W-Cu composite powder is divided to sinter at the same temperature near complete fine and close；
(3) method using place Min layers powder compressing will obtain nano combined W-Cu powder in step (2)
It is pressed into the W-Cu material pressed compact with gradient-structure；
(4) the pressed compact pre-burning in protective atmosphere that will obtain in step (3)；
(5) base substrate high temperature one step in protective atmosphere after obtaining pre-burning in step (4) sinters, it is thus achieved that
Coating combination is intact, be combined W-Cu material close to fully dense nanometer gradient.
Nanometer gradient the most according to claim 1 is combined the preparation method of W-Cu material, and its feature exists
In, described step (2) nano combined W-Cu powder uses colloidal sol-spray drying-thermal reduction technology, machinery
Prepared by one or more in alloying and sol-gel process, in powder preparing processes:
(1) colloidal sol-spray drying-thermal reduction prepares nano combined W-Cu powder: copper content is at 10-30wt.%
W-Cu composite powder calcining heat control at 400-500 DEG C, reduction temperature controls at 600-750 DEG C, reduction
Time is at 1-2h；
Copper content controls at 500-700 DEG C in the W-Cu composite powder calcining heat of 30-40wt.%, reduction temperature
Degree controls at 750-850 DEG C, and the recovery time is at 2-3h；
Copper content controls at 700-800 DEG C in the W-Cu composite powder calcining heat of 40-60wt.%, reduction temperature
Degree controls at 800-900 DEG C, and the recovery time is at 3-4h；
(2) nano combined W-Cu powder is prepared in mechanical alloying: copper content is multiple at the W-Cu of 10-30wt.%
Closing powder ratio of grinding media to material is 10-20:1, and rotating speed is 400-500r/min, and Ball-milling Time is 40-60 hour；
Copper content is 5-15:1 in the W-Cu composite powder ratio of grinding media to material of 30-40wt.%, and rotating speed is 300-400r/min,
Ball-milling Time is 20-40 hour；
Copper content is 5-10:1 in the W-Cu composite powder ratio of grinding media to material of 40-60wt.%, and rotating speed is 300-350r/min,
Ball-milling Time is 10-20 hour；
Various composite powders use argon to be that protective gas prevents Powder Oxidation, with dehydrated alcohol in mechanical milling process
Wet grinding is carried out for solvent；
(3) sol-gel process prepares nano combined W-Cu powder: copper content is at the W-Cu of 10-30wt.%
In composite powder solution, solute ratio is at 10-20wt%, and calcining heat is at 300-400 DEG C, and reduction temperature exists
500-600 DEG C, the recovery time is at 1-2h；
Solute ratio is at 20-30wt% in the W-Cu composite powder solution of 30-40wt.% for copper content, and calcining is warm
Degree is at 400-500 DEG C, and reduction temperature is at 600-700 DEG C, and the recovery time is at 2-3h；
Solute ratio is at 30-40wt% in the W-Cu composite powder solution of 40-60wt.% for copper content, and calcining is warm
Degree is at 500-600 DEG C, and reduction temperature is at 700-800 DEG C, and the recovery time is at 3-4h.
Nanometer gradient the most according to claim 1 is combined the preparation method of W-Cu material, and its feature exists
In, the method that place Min layers powder described in step (3) is compressing, including procedure below:
After nano combined W-Cu powder is pressed copper content place Min layers powder the most successively compressing；
The powder completed is suppressed at 100-400MPa, pressurize 5-10s.
Nanometer gradient the most according to claim 1 is combined the preparation method of W-Cu material, and its feature exists
In, the burn-in process described in step (4) is: in hydrogen or nitrogen or vacuum atmosphere, 500～1000 DEG C
Pre-burning 0.5-3h.
Nanometer gradient the most according to claim 1 is combined the preparation method of W-Cu material, and its feature exists
In, the high temperature one step sintering described in step (5), refer in hydrogen or nitrogen or vacuum atmosphere,
1300～1450 DEG C of one step sintering 0.5-3h.
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Cited By (6)
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| CN106825583A (en) * | 2016-12-30 | 2017-06-13 | 中南大学 | A kind of tungsten and low activation stainless steel nanometer gradient composite connecting method |
| CN107604188A (en) * | 2017-09-18 | 2018-01-19 | 北京科技大学 | A kind of method for preparing gradient porous tungsten |
| CN109680177A (en) * | 2019-03-04 | 2019-04-26 | 合肥工业大学 | A kind of plating W diamond/W-Cu gradient composites preparation method |
| CN111809093A (en) * | 2020-07-21 | 2020-10-23 | 广东正信硬质材料技术研发有限公司 | Wear-resistant hard alloy and preparation method thereof |
| CN112091217A (en) * | 2020-11-12 | 2020-12-18 | 陕西斯瑞新材料股份有限公司 | Method for manufacturing copper-tungsten material by adopting spherical tungsten powder laser 3D printing |
| CN114990404A (en) * | 2022-07-01 | 2022-09-02 | 合肥工业大学 | AlN/W-Cu layered gradient composite material and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106825583A (en) * | 2016-12-30 | 2017-06-13 | 中南大学 | A kind of tungsten and low activation stainless steel nanometer gradient composite connecting method |
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| CN109680177A (en) * | 2019-03-04 | 2019-04-26 | 合肥工业大学 | A kind of plating W diamond/W-Cu gradient composites preparation method |
| CN109680177B (en) * | 2019-03-04 | 2020-12-29 | 合肥工业大学 | Preparation method of W-plated diamond/W-Cu gradient composite material |
| CN111809093A (en) * | 2020-07-21 | 2020-10-23 | 广东正信硬质材料技术研发有限公司 | Wear-resistant hard alloy and preparation method thereof |
| CN112091217A (en) * | 2020-11-12 | 2020-12-18 | 陕西斯瑞新材料股份有限公司 | Method for manufacturing copper-tungsten material by adopting spherical tungsten powder laser 3D printing |
| CN112091217B (en) * | 2020-11-12 | 2021-02-09 | 陕西斯瑞新材料股份有限公司 | Method for manufacturing copper-tungsten material by adopting spherical tungsten powder laser 3D printing |
| CN114990404A (en) * | 2022-07-01 | 2022-09-02 | 合肥工业大学 | AlN/W-Cu layered gradient composite material and preparation method thereof |
| CN114990404B (en) * | 2022-07-01 | 2022-12-27 | 合肥工业大学 | AlN/W-Cu layered gradient composite material and preparation method thereof |
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