CN109022870A - A kind of high rigidity PCD composite sheet and preparation method thereof - Google Patents
A kind of high rigidity PCD composite sheet and preparation method thereof Download PDFInfo
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- CN109022870A CN109022870A CN201811022039.8A CN201811022039A CN109022870A CN 109022870 A CN109022870 A CN 109022870A CN 201811022039 A CN201811022039 A CN 201811022039A CN 109022870 A CN109022870 A CN 109022870A
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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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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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
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
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Abstract
The invention discloses a kind of high rigidity PCD composite sheets and preparation method thereof, the preparation method includes: 1) to disperse nano silica, hydrochloric acid in the aqueous solution of alcohol, it is subsequently added into sodium salt, aluminium salt, boric acid, zirconates, yttrium salt, nickel salt, butyl titanate mixing, then lye is added dropwise and stirs, is finally aged, is dry to obtain xerogel；2) xerogel is heat-treated to obtain heat-treated products；3) heat-treated products, zinc powder, cobalt powder, glass putty and barium powder are subjected to ball milling to obtain bonding agent；4) by diamond dust, bonding agent in 1600-1800 DEG C, 2 × 1011Pa‑10×1011Sintering is under Pa to be made the high rigidity PCD composite sheet.PCD composite sheet of the present invention has excellent hardness, while the preparation method has the advantages that process is simply and easy to operate.
Description
Technical field
The present invention relates to PCD cutters, and in particular, to a kind of high rigidity PCD composite sheet and its preparation side.
Background technique
Diamond is applied to machining as a kind of ultrahard cutting tool material and has centuries history.Cutter development course,
From late nineteenth century to the twentieth century phase, cutter material is using high-speed steel as main representative；Nineteen twenty-seven, Germany developed hard first
Alloy cutter material is simultaneously widely applied；Nineteen fifties, the U.S. of Sweden are respectively synthesized out diamond, cutting
It is to represent period that cutter, which is stepped into from this with superhard material,.Nineteen seventies, people are synthesized using high-pressure synthesis technology
Polycrystalline diamond (PCD) solves the problems, such as natural diamond rare numbers, expensive, expands diamond cutter application range
Open up the multiple fields such as Aeronautics and Astronautics, automobile, electronics, stone material.
Diamond cutter has the characteristics such as hardness is high, compression strength is high, thermal conductivity and wearability are good, can high-speed cutting acquisition
Very high manufacturing accuracy processing efficiency.The above-mentioned characteristic of diamond cutter is determined by diamond crystal state.Diamond crystal, carbon atom
Four valence electrons press tetrahedral structure bonding, and each carbon atom and four adjacent atoms form covalent bond, and then form diamond
Structure, the structure binding force directionality is very strong, so that diamond be made to have extreme hardness.Since polycrystalline diamond PCD structure takes
To different fine-particle diamond sintered body, although joined bonding agent, hardness and wearability are still below single-crystal diamond.
Summary of the invention
The object of the present invention is to provide a kind of high rigidity PCD composite sheet and preparation method thereof, which has excellent
Hardness, while the preparation method have the advantages that process simply and it is easy to operate.
To achieve the goals above, the present invention provides a kind of preparation methods of high rigidity PCD composite sheet, comprising:
1) disperse nano silica, hydrochloric acid in the aqueous solution of alcohol, be subsequently added into sodium salt, aluminium salt, boric acid, zirconates, yttrium salt,
Then nickel salt, butyl titanate mixing are added dropwise lye and stir, be finally aged, be dry to obtain xerogel；
2) xerogel is heat-treated to obtain heat-treated products；
3) heat-treated products, zinc powder, cobalt powder, glass putty and barium powder are subjected to ball milling to obtain bonding agent；
4) by diamond dust, bonding agent in 1600-1800 DEG C, 2 × 1011Pa-10×1011Sintering is under Pa to be made the height
Hardness PCD composite sheet.
The present invention also provides a kind of high rigidity PCD composite sheet, high rigidity PCD composite sheet passes through above-mentioned preparation method
It is prepared.
In above-mentioned technical proposal, the present invention pass through first sol-gel method be made xerogel, then by heat treatment so that
Xerogel resolves into the complex being made of many oxide, finally by heat-treated products, zinc powder, cobalt powder, glass putty and barium powder
It is combined to form bonding agent, finally bonding agent, diamond dust is calcined, high rigidity PCD composite sheet is made；The bonding agent energy
Enough so that PCD composite sheet obtained has excellent hardness, while the preparation method has process simply and easy to operate excellent
Point.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of preparation methods of high rigidity PCD composite sheet, comprising:
1) disperse nano silica, hydrochloric acid in the aqueous solution of alcohol, be subsequently added into sodium salt, aluminium salt, boric acid, zirconates, yttrium salt,
Then nickel salt, butyl titanate mixing are added dropwise lye and stir, be finally aged, be dry to obtain xerogel；
2) xerogel is heat-treated to obtain heat-treated products；
3) heat-treated products, zinc powder, cobalt powder, glass putty and barium powder are subjected to ball milling to obtain bonding agent；
4) by diamond dust, bonding agent in 1600-1800 DEG C, 2 × 1011Pa-10×1011Sintering is under Pa to be made the height
Hardness PCD composite sheet.
In step 1) of the invention, the dosage of each material can select in a wide range, but in order to further mention
The hardness of PCD composite sheet made from height, it is preferable that in step 1), nano silica, sodium salt, aluminium salt, boric acid, zirconates, yttrium
Salt, nickel salt, butyl titanate molar ratio be 1:0.4-0.6:0.7-0.9:0.2-0.4:0.05-0.15:0.08-0.12:
0.1-0.3:0.25-0.35.
In step 1) of the invention, hydrochloric acid, the aqueous solution of alcohol, lye dosage can select in a wide range, but
It is the hardness in order to further increase PCD composite sheet obtained, it is preferable that in step 1), nano silica, hydrochloric acid, alcohol
Aqueous solution, lye amount ratio be 1mmol:2-3mL:5-10mL:4-6mL, and the volume fraction of alcohol is in the aqueous solution of alcohol
30-40%, the pH of hydrochloric acid are 4-5, and the pH of lye is 11-13.
In step 1) of the invention, the type of each material can select in a wide range, but in order to further mention
The hardness of PCD composite sheet made from height, it is preferable that in step 1), the alcohol of the aqueous solution of alcohol be selected from ethyl alcohol, methanol, propyl alcohol and
At least one of isopropanol；Lye is selected from least one of potassium hydroxide aqueous solution, sodium hydrate aqueous solution；Sodium salt is selected from
At least one of sodium chloride, sodium sulphate, sodium nitrate；Aluminium salt is selected from least one of aluminum nitrate, aluminium chloride, aluminum acetate；Zirconium
Salt is selected from least one of zirconium nitrate, citric acid zirconates；Yttrium salt is selected from yttrium nitrate, three (radical) yttrium salts, fluoroform
At least one of sulfonic acid yttrium；Nickel salt is selected from least one of nickel nitrate, nickel sulfate, nickel chloride.
In step 1) of the invention, the condition of ageing can select in a wide range, but in order to further increase
The hardness of PCD composite sheet obtained, it is preferable that in step 1), ageing meets the following conditions: Aging Temperature is 25-35 DEG C, old
The change time is 18-24h.
In step 1) of the invention, dry condition can select in a wide range, but in order to further increase
Preferably, in step 1), drying meets the following conditions to the hardness of PCD composite sheet obtained: drying temperature is 100-110 DEG C,
Drying time is 2-4h.
In step 1) of the invention, the mixed time can select in a wide range, but in order to further increase
The hardness of PCD composite sheet obtained, it is preferable that in step 1), the mixed time is 15-20min.
In step 2) of the invention, the condition of heat treatment can select in a wide range, but in order to further mention
The hardness of PCD composite sheet made from height, it is preferable that in step 2, heat treatment meets the following conditions: treatment temperature 510-
530 DEG C, the processing time is 6-10h.
In step 3) of the invention, the dosage of each material can select in a wide range, but in order to further mention
The hardness of PCD composite sheet made from height, it is preferable that in step 3), heat-treated products, zinc powder, cobalt powder, glass putty and barium powder weight
Amount is than being 10:1-3:0.8-1.3:2.1-2.6:1.2-1.6.
In step 3) of the invention, the condition of ball milling can select in a wide range, but in order to further increase
The hardness of PCD composite sheet obtained, it is preferable that in step 3), ball milling meets the following conditions: the mass ratio of abrading-ball and material is
20:0.8-1.2 revolving speed 1600-1800rpm, Ball-milling Time 40-60min.
In step 4) of the invention, the time of calcining can select in a wide range, but in order to further increase
The hardness of PCD composite sheet obtained, it is preferable that in step 4), the time of calcining is 12-15h；
In step 4) of the invention, the granularity of diamond dust can select in a wide range, but in order to further mention
The hardness of PCD composite sheet made from height, it is preferable that in step 4), the granularity of diamond dust is 2-4 μm.
The present invention also provides a kind of high rigidity PCD composite sheet, high rigidity PCD composite sheet passes through above-mentioned preparation method
It is prepared.
The present invention will be described in detail by way of examples below.
Embodiment 1
1) it disperses nano silica, hydrochloric acid in the aqueous solution of alcohol (ethyl alcohol), is subsequently added into sodium salt (sodium chloride), aluminium salt
(aluminum nitrate), boric acid, zirconates (zirconium nitrate), yttrium salt (yttrium nitrate), nickel salt (nickel nitrate), butyl titanate mixing 18min, then
Lye (potassium hydroxide aqueous solution) is added dropwise and stirs 18min, finally ageing (Aging Temperature is 30 DEG C, digestion time 20h) is done
Dry (drying temperature is 105 DEG C, drying time 3h) is to obtain xerogel；Wherein, nano silica, sodium salt, aluminium salt, boron
Acid, zirconates, yttrium salt, nickel salt, butyl titanate molar ratio be 1:0.5:0.8:0.3:0.1:0.1:0.2:0.30；Nano-silica
SiClx, hydrochloric acid, the aqueous solution of alcohol, lye amount ratio be 1mmol:2.5mL:8mL:5mL, and alcohol in the aqueous solution of the alcohol
Volume fraction is 35%, and the pH of the hydrochloric acid is 4.5, and the pH of the lye is 12；
2) xerogel is heat-treated (treatment temperature is 520 DEG C, and the processing time is 8h) to obtain heat-treated products；
3) by heat-treated products, zinc powder, cobalt powder, glass putty and barium powder according to the weight ratio row ball milling (abrading-ball of 10:2:1:2.3:1.4
Mass ratio with material is 20:1, revolving speed 1700rpm, Ball-milling Time 50min) to obtain bonding agent A1.
Embodiment 2
1) it disperses nano silica, hydrochloric acid in the aqueous solution of alcohol (propyl alcohol), is subsequently added into sodium salt (sodium sulphate), aluminium salt
(aluminium chloride), boric acid, zirconates (citric acid zirconates), yttrium salt (three (radical) yttrium salts), nickel salt (nickel sulfate), butyl titanate
15min is mixed, lye (sodium hydrate aqueous solution) is then added dropwise and stirs 15min, (Aging Temperature is 25 DEG C, old for finally ageing
Changing the time is for 24 hours), dry (drying temperature is 100 DEG C, drying time 4h) to obtain xerogel；Wherein, nanometer titanium dioxide
Silicon, sodium salt, aluminium salt, boric acid, zirconates, yttrium salt, nickel salt, butyl titanate molar ratio be 1:0.4:0.7:0.2:0.05:0.08:
0.1:0.25；Nano silica, hydrochloric acid, the aqueous solution of alcohol, lye amount ratio be 1mmol:2mL:5mL:4mL, and it is described
The volume fraction of alcohol is 30% in the aqueous solution of alcohol, and the pH of the hydrochloric acid is 4, and the pH of the lye is 11；
2) xerogel is heat-treated (treatment temperature is 510 DEG C, and the processing time is 10h) to obtain heat-treated products；
3) by heat-treated products, zinc powder, cobalt powder, glass putty and barium powder according to the weight ratio row ball milling (mill of 10:1:0.8:2.1:1.2
The mass ratio of ball and material is 20:0.8, revolving speed 1600rpm, Ball-milling Time 60min) to obtain bonding agent A2.
Embodiment 3
1) it disperses nano silica, hydrochloric acid in the aqueous solution of alcohol (isopropanol), is subsequently added into sodium salt (sodium nitrate), aluminium salt
(aluminum acetate), boric acid, zirconates (citric acid zirconates), yttrium salt (trifluoromethayl sulfonic acid yttrium), nickel salt (nickel chloride), butyl titanate are mixed
20min is closed, lye (sodium hydrate aqueous solution) is then added dropwise and stirs 20min, (Aging Temperature is 35 DEG C, ageing for finally ageing
Time is 18h), dry (drying temperature is 110 DEG C, drying time 2h) to obtain xerogel；Wherein, nano silica,
Sodium salt, aluminium salt, boric acid, zirconates, yttrium salt, nickel salt, butyl titanate molar ratio be 1:0.6:0.9:0.4:0.15:0.12:
0.3:0.35；Nano silica, hydrochloric acid, the aqueous solution of alcohol, lye amount ratio be 1mmol:3mL:10mL:6mL, and it is described
The volume fraction of alcohol is 40% in the aqueous solution of alcohol, and the pH of the hydrochloric acid is 5, and the pH of the lye is 13；
2) xerogel is heat-treated (treatment temperature is 530 DEG C, and the processing time is 6h) to obtain heat-treated products；
3) by heat-treated products, zinc powder, cobalt powder, glass putty and barium powder according to the weight ratio row ball milling (mill of 10:3:1.3:2.6:1.6
The mass ratio of ball and material is 20:1.2, revolving speed 1800rpm, Ball-milling Time 40min) to obtain bonding agent A3.
Application examples 1
By granularity be 2 μm of diamond dusts, above-mentioned bonding agent according to the weight ratio of 1:5 in 1700 DEG C, 6 × 1011It is sintered under Pa
Then 13h detects the hardness of PCD composite sheet, the results are shown in Table 1 so that high rigidity PCD composite sheet is made.
Table 1
| Bonding agent | A1 | A2 | A3 |
| Hardness/HV | 8657 | 8669 | 8642 |
The preferred embodiment of the present invention has been described above in detail, still, the tool during present invention is not limited to the embodiments described above
Body details within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, these letters
Monotropic type all belongs to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (9)
1. a kind of preparation method of high rigidity PCD composite sheet characterized by comprising
1) disperse nano silica, hydrochloric acid in the aqueous solution of alcohol, be subsequently added into sodium salt, aluminium salt, boric acid, zirconates, yttrium salt,
Then nickel salt, butyl titanate mixing are added dropwise lye and stir, be finally aged, be dry to obtain xerogel；
2) xerogel is heat-treated to obtain heat-treated products；
3) heat-treated products, zinc powder, cobalt powder, glass putty and barium powder are subjected to ball milling to obtain bonding agent；
4) by diamond dust, bonding agent in 1600-1800 DEG C, 2 × 1011Pa-10×1011It is sintered under Pa to be made described high hard
Spend PCD composite sheet.
2. preparation method according to claim 1, wherein in step 1), the nano silica, sodium salt, aluminium salt,
Boric acid, zirconates, yttrium salt, nickel salt, butyl titanate molar ratio be 1:0.4-0.6:0.7-0.9:0.2-0.4:0.05-0.15:
0.08-0.12:0.1-0.3:0.25-0.35.
3. preparation method according to claim 1, wherein in step 1), the nano silica, hydrochloric acid, alcohol
Aqueous solution, lye amount ratio be 1mmol:2-3mL:5-10mL:4-6mL, and in the aqueous solution of the alcohol alcohol volume fraction
It is 4-5 for 30-40%, the pH of the hydrochloric acid, the pH of the lye is 11-13.
4. preparation method according to claim 1, wherein in step 1), the alcohol of the aqueous solution of the alcohol be selected from ethyl alcohol,
At least one of methanol, propyl alcohol and isopropanol；The lye in potassium hydroxide aqueous solution, sodium hydrate aqueous solution extremely
Few one；The sodium salt is selected from least one of sodium chloride, sodium sulphate, sodium nitrate；The aluminium salt is selected from aluminum nitrate, chlorination
At least one of aluminium, aluminum acetate；The zirconates is selected from least one of zirconium nitrate, citric acid zirconates；The yttrium salt is selected from
At least one of yttrium nitrate, three (radical) yttrium salts, trifluoromethayl sulfonic acid yttrium；The nickel salt be selected from nickel nitrate, nickel sulfate,
At least one of nickel chloride.
5. preparation method according to claim 1, wherein in step 1), the ageing meets the following conditions: ageing temperature
Degree is 25-35 DEG C, digestion time 18-24h；
Preferably, in step 1), the drying meets the following conditions: drying temperature is 100-110 DEG C, drying time 2-
4h；
Preferably, in step 1), the mixed time is 15-20min.
6. preparation method according to claim 1, wherein in step 2, the heat treatment meets the following conditions: processing
Temperature is 510-530 DEG C, and the processing time is 6-10h.
7. preparation method according to claim 1, wherein in step 3), the heat-treated products, zinc powder, cobalt powder, tin
The weight ratio of powder and barium powder is 10:1-3:0.8-1.3:2.1-2.6:1.2-1.6.
8. preparation method according to claim 1, wherein in step 3), the ball milling meets the following conditions: abrading-ball with
The mass ratio of material is 20:0.8-1.2, revolving speed 1600-1800rpm, Ball-milling Time 40-60min；
Preferably, in step 4), the time of the calcining is 12-15h；
It is highly preferred that the granularity of the diamond dust is 2-4 μm in step 4).
9. a kind of high rigidity PCD composite sheet, which is characterized in that the high rigidity PCD composite sheet passes through any in claim 1-8
Preparation method described in one is prepared.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811022039.8A CN109022870A (en) | 2018-09-04 | 2018-09-04 | A kind of high rigidity PCD composite sheet and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811022039.8A CN109022870A (en) | 2018-09-04 | 2018-09-04 | A kind of high rigidity PCD composite sheet and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3785825A1 (en) * | 2019-08-30 | 2021-03-03 | 3M Innovative Properties Company | Powder blend for use in additive manufacturing |
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2018
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3785825A1 (en) * | 2019-08-30 | 2021-03-03 | 3M Innovative Properties Company | Powder blend for use in additive manufacturing |
| WO2021038465A1 (en) * | 2019-08-30 | 2021-03-04 | 3M Innovative Properties Company | Powder blend for use in additive manufacturing |
| CN114286729A (en) * | 2019-08-30 | 2022-04-05 | 3M创新有限公司 | Powder blend for laminate manufacturing |
| CN114286729B (en) * | 2019-08-30 | 2024-01-02 | 3M创新有限公司 | Powder blend for layup manufacture |
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