CN103755317A - Preparation method of strengthened polycrystalline cubic boron nitride composite super-hard material - Google Patents
Preparation method of strengthened polycrystalline cubic boron nitride composite super-hard material Download PDFInfo
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- CN103755317A CN103755317A CN201410025088.2A CN201410025088A CN103755317A CN 103755317 A CN103755317 A CN 103755317A CN 201410025088 A CN201410025088 A CN 201410025088A CN 103755317 A CN103755317 A CN 103755317A
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- boron nitride
- cubic boron
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- superhard material
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Abstract
The invention discloses a method for preparing a strengthened polycrystalline cubic boron nitride (PCBN) composite super-hard material by adding strengthened phases of super-hard materials such as cubic boron nitride c-BC2N, boron nitride (B4C) and nanometer twin crystal cubic boron nitride (nt-CBN) into a PCBN material, relating to a novel method for synthesizing a super-hard composite material by means of high-temperature and high-pressure sintering, and belongs to the field of super-hard materials. The method comprises the following steps: cutting a super-high-hardness material into a strengthened stem body; burying the strengthened stem body into powder, placing a pyrophyllite block and synthesizing under a high-temperature and high-pressure condition to obtain the PCBN material with a strengthened core. The strengthened PCBN composite super-hard material prepared by using the method has the toughness of PCBN as well as super high hardness which is comparable to that of a natural diamond material. The problems of higher and higher requirements on tools in the modern machining industry and the awkward situation of the application of certain super-high-hardness materials are solved, and the application field of the super-hard material is expanded.
Description
Technical field
The synthetic method that the present invention relates to a kind of polycrystalline cubic boron nitride composite superhard material that has added superhard material wild phase under High Temperature High Pressure, belongs to superhard material field.
Background technology
Polycrystalline cubic boron nitride (PCBN) is a kind of take fine cubic boron nitride as raw material and add the superhard agglomerate that a certain amount of caking agent sintering under high-temperature and high-pressure conditions forms.
Because PCBN has multiple excellent properties, as ultrahigh hardness and wear resistance, high thermostability, extremely strong chemical stability and good heat conductivility etc., make it there is long work-ing life and high working accuracy and be widely used in field of machining, as high-precision systems such as numerically-controlled machine, multiple purpose machine, automation line, specialized high-speed lathe, flcxible production unit or flexible manufacturing systems, or for the manufacture field of the difficult-to-machine materials such as cutting alloy steel, tool steel, spray material.
But along with the development of modern industry, the difficulty of processing of novel material is increasing, existing PCBN cutter shows the tired state of processing gradually.
Existing its hardness of some material is the highest in current nature or synthetic product, but has limited its range of application because of its high fragility, as a cube boron carbonitrides c-BC
2n, norbide B
4c and nano twin crystal cubic boron nitride nt-CBN etc.
At present, mechanical processing industry is more and more higher to the requirement of PCBN cutter, and the superhard material that some fragility is high simultaneously is also faced with certain difficult situation in application.
Summary of the invention
The technical issues that need to address of the present invention are just to overcome the defect of prior art, a kind of preparation method who strengthens polycrystalline cubic boron nitride composite superhard material is provided, strengthening PCBN composite superhard material prepared by the present invention is with the toughness of PCBN, ultrahigh hardness with the natural diamond material that matches in excellence or beauty, solved modern mechanical processing industry to the more and more higher requirement of cutter and some utmost point superhard materials difficult situation in application aspect, widened the Application Areas of superhard material.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of preparation method who strengthens polycrystalline cubic boron nitride composite superhard material, described method comprises the following steps:
A, prepare superhard material and strengthen core: adopt laser cutting technique that enhancings core superhard material is cut into enhancing stem stem body;
B, powder configuration:
Cubic boron nitride cBN carries out purification process, and caking agent carries out mechanical ball milling in vacuum sphere grinding machine;
According to cBN, account for the ratio that total mixed powder mass ratio is 60-90% and mix cBN and caking agent, mixed powder packs in graphite matrix, puts into one or more enhancing stem stem bodies, vacuum reducing;
C, synthetic: graphite assembly is put into pyrophyllite block and assemble, the pyrophyllite block that assembling is completed is put into press, at high pressure 70-100MPa, the synthetic PCBN composite superhard material that contains wild phase under the synthesis condition of heating current 40-55A;
D, aftertreatment: the PCBN composite superhard material that contains wild phase obtaining is carried out to aftertreatment.
In the present invention, described enhancing core superhard material is a cube boron carbonitrides c-BC
2n, norbide B
4one or more in C or nano twin crystal cubic boron nitride nt-CBN.
In the present invention, cBN purification step is carried out acid treatment for first carrying out after alkaline purification; Alkaline purification is for being that 1:1 ratio and cBN mix and put into retort furnace and be incubated at 350 ℃ after 1 hour naturally cooling and repeatedly rinse to neutrality with hot water by solid NaOH or KOH according to weight ratio; Acid treatment is that alkaline purification cBN is later poured in large volume beaker and adds higher than the nitric acid of cBN 2-3cm and boil 20 minutes, adds hydrochloric acid to boil 20 minutes after outwelling nitric acid, is washed till neutrality with distilled water.
In the present invention, pack into and strengthen stem stem body step and make to strengthen stem stem body and have more than 70% surface-area in mixing under powder parcel.
In the present invention, the vacuum sphere time consuming of caking agent is greater than 24h.
In the present invention, the time of vacuum reducing is greater than 24h.
In the present invention, aftertreatment is pickling after pickling or ball milling.
In the present invention, the cross section of described enhancing stem stem body is circular, square or trilateral.
Beneficial effect of the present invention is: strengthening PCBN composite superhard material prepared by the present invention is with the toughness of PCBN, ultrahigh hardness with the natural diamond material that matches in excellence or beauty, solved modern mechanical processing industry to the more and more higher requirement of cutter and some utmost point superhard materials difficult situation in application aspect, widened the Application Areas of superhard material.
Accompanying drawing explanation
Fig. 1 is that a kind of external parcel body shell is the columniform PCBN composite superhard material that has added wild phase.
Reference numeral: 1 for strengthening core square column; 2 is outer inclusion, i.e. PCBN.
Embodiment
embodiment 1:
1, utilize laser cutting machine that a cube boron carbonitrides is cut into the little square column of 1 × 1 × 4mm.
2, powder configuration:
According to granularity, be that 1-2 μ m, 5-10 μ m, its quality proportion of 20-30 μ m ratio of 15%, 25%, 60% of being respectively is carried out proportioning to cBN; CBN is carried out to purification process, first carry out carrying out acid treatment after alkaline purification; Alkaline purification is for being that 1:1 ratio and cBN mix and put into retort furnace and be incubated at 350 ℃ after 1 hour naturally cooling and repeatedly rinse to neutrality with hot water by solid NaOH or KOH according to weight ratio; Acid treatment is that alkaline purification cBN is later poured in large volume beaker and adds higher than the nitric acid of cBN 2-3cm and boil 20 minutes, adds more hydrochloric acid to boil 20 minutes after outwelling nitric acid, is washed till neutrality with distilled water.
By Al and Al
2o
3, SiC is that 2:1:1 ratio is mixed as caking agent according to weight ratio, caking agent carries out mechanical treatment, ball milling 36h in vacuum sphere grinding machine;
According to cBN, total powder quality is mixed to cBN and caking agent than the ratio that is 80%, mixed powder packs into be put into 1 superhard material and strengthens core in graphite matrix, and strengthening stem stem body has more than 70% surface-area under powder parcel.Vacuum reducing 24h;
3, graphite molectron is put into pyrophyllite block and assemble, the pyrophyllite block that assembling is completed is put into press, at high pressure 80MPa, and the synthetic PCBN composite superhard material that strengthens core that contains under the synthesis technique of heating current 45A;
4, by what obtain, containing cube boron carbonitrides, strengthen pickling after the PCBN super-hard material ball milling of core.
embodiment 2:
1, utilize laser cutting machine that norbide is cut into Φ 1 × 4mm small column.
2, powder configuration:
According to granularity, be that 1-2 μ m, 5-10 μ m, its quality proportion of 20-30 μ m ratio of 10%, 30%, 60% of being respectively is carried out proportioning to cBN; CBN is carried out to purification process, first carry out carrying out acid treatment after alkaline purification; Alkaline purification is for being that 1:1 ratio and cBN mix and put into retort furnace and be incubated at 350 ℃ after 1 hour naturally cooling and repeatedly rinse to neutrality with hot water by solid NaOH or KOH according to weight ratio; Acid treatment is that alkaline purification cBN is later poured in large volume beaker and adds higher than the nitric acid of cBN 2-3cm and boil 20 minutes, adds more hydrochloric acid to boil 20 minutes after outwelling nitric acid, is washed till neutrality with distilled water.
Al and SiC are mixed as caking agent according to 1:1 ratio, and caking agent carries out mechanical treatment, ball milling 48h in vacuum sphere grinding machine;
The ratio that is 80% to total mixed powder mass ratio according to cBN mixes cBN and caking agent, and mixed powder packs in graphite matrix puts into 1 superhard material enhancing core, strengthens stem stem body completely under powder parcel.Vacuum reducing 36h.
3, graphite molectron is put into pyrophyllite block and assemble, the pyrophyllite block that assembling is completed is put into press, at high pressure 70MPa, and the synthetic PCBN composite superhard material that strengthens core that contains under the synthesis technique of heating current 40A;
4, by pickling after the PCBN super-hard material ball milling that contains norbide enhancing core obtaining.
embodiment 3:
1, utilize laser cutting machine that nano twin crystal cubic boron nitride is cut into the length of side for 1.2mm, height is the triangular prism of 4mm;
2, powder configuration:
According to granularity, be that 1-2 μ m, 5-10 μ m, its quality proportion of 20-30 μ m ratio of 12%, 32%, 56% of being respectively is carried out proportioning to cBN; CBN is carried out to purification process, first carry out carrying out acid treatment after alkaline purification; Alkaline purification is for being that 1:1 ratio and cBN mix and put into retort furnace and be incubated at 350 ℃ after 1 hour naturally cooling and repeatedly rinse to neutrality with hot water by solid NaOH or KOH according to weight ratio; Acid treatment is that alkaline purification cBN is later poured in large volume beaker and adds higher than the nitric acid of cBN 2-3cm and boil 20 minutes, adds more hydrochloric acid to boil 20 minutes after outwelling nitric acid, is washed till neutrality with distilled water.
By Al, Ti and SiC, Al
4n
3according to weight ratio 1:1:1:1 ratio, mix as caking agent, caking agent carries out mechanical treatment, ball milling 36h in vacuum sphere grinding machine;
According to cBN, total powder quality is mixed to cBN and caking agent than the ratio that is 90%, mixed powder packs in graphite matrix puts into 2 superhard materials enhancing cores, strengthens stem stem body completely under powder parcel.Vacuum reducing 24h;
3, graphite molectron is put into pyrophyllite block and assemble, the pyrophyllite block that assembling is completed is put into press, at high pressure 100MPa, and the synthetic PCBN composite superhard material that strengthens core that contains under the synthesis technique of heating current 50A;
4, by pickling after the PCBN super-hard material ball milling that contains nano twin crystal cubic boron nitride enhancing core obtaining.
embodiment 4:
1, utilize laser cutting machine that nano twin crystal cubic boron nitride is cut into the little square column of Φ 1 × 5mm, a cube boron carbonitrides is cut into the little square column of Φ 1 × 5mm.
2, powder configuration:
According to granularity, be that 1-2 μ m, 5-10 μ m, its quality proportion of 20-30 μ m ratio of 15%, 20%, 65% of being respectively is carried out proportioning to cBN; CBN is carried out to purification process, first carry out carrying out acid treatment after alkaline purification; Alkaline purification is for being that 1:1 ratio and cBN mix and put into retort furnace and be incubated at 350 ℃ after 1 hour naturally cooling and repeatedly rinse to neutrality with hot water by solid NaOH or KOH according to weight ratio; Acid treatment is that alkaline purification cBN is later poured in large volume beaker and adds higher than the nitric acid of cBN 2-3cm and boil 20 minutes, adds more hydrochloric acid to boil 20 minutes after outwelling nitric acid, is washed till neutrality with distilled water.
Al, Ti and SiC, Al4N3 are mixed as caking agent according to weight ratio 1:1:1:1 ratio, and caking agent carries out mechanical treatment, ball milling 40h in vacuum sphere grinding machine;
According to cBN, total powder quality is mixed to cBN and caking agent than the ratio that is 90%, mixed powder packs interval 0.5mm in graphite matrix into and puts into 1 cube of boron carbonitrides and 1 nano twin crystal cubic boron nitride pillar, and strengthening stem stem body has more than 70% surface-area under powder parcel.Vacuum reducing 24h;
3, graphite molectron is put into pyrophyllite block and assemble, the pyrophyllite block that assembling is completed is put into press, at high pressure 85MPa, and the synthetic PCBN composite superhard material that strengthens core that contains under the synthesis technique of heating current 55A;
4, by pickling after the PCBN super-hard material ball milling that contains nano twin crystal cubic boron nitride and cube boron carbonitrides enhancing core obtaining.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.And the apparent variation of being amplified out thus or variation are still among protection scope of the present invention.
Claims (8)
1. a preparation method who strengthens polycrystalline cubic boron nitride composite superhard material, is characterized in that, described method comprises the following steps:
A, prepare superhard material and strengthen core: adopt laser cutting technique that enhancings core superhard material is cut into enhancing stem stem body;
B, powder configuration:
Cubic boron nitride cBN carries out purification process, and caking agent carries out mechanical ball milling in vacuum sphere grinding machine;
According to cBN, account for the ratio that total mixed powder mass ratio is 60-90% and mix cBN and caking agent, mixed powder packs in graphite matrix, puts into one or more enhancing stem stem bodies, vacuum reducing;
C, synthetic: graphite assembly is put into pyrophyllite block and assemble, the pyrophyllite block that assembling is completed is put into press, at high pressure 70-100MPa, the synthetic PCBN composite superhard material that contains wild phase under the synthesis condition of heating current 40-55A;
D, aftertreatment: the PCBN composite superhard material that contains wild phase obtaining is carried out to aftertreatment.
2. the preparation method of strengthening polycrystalline cubic boron nitride composite superhard material as claimed in claim 1, is characterized in that, described enhancing core superhard material is a cube boron carbonitrides c-BC
2n, norbide B
4one or more in C or nano twin crystal cubic boron nitride nt-CBN.
3. the preparation method of strengthening polycrystalline cubic boron nitride composite superhard material as claimed in claim 1, is characterized in that, cBN purification step is carried out acid treatment for first carrying out after alkaline purification; Alkaline purification is for being that 1:1 ratio and cBN mix and put into retort furnace and be incubated at 350 ℃ after 1 hour naturally cooling and repeatedly rinse to neutrality with hot water by solid NaOH or KOH according to weight ratio; Acid treatment is that alkaline purification cBN is later poured in large volume beaker and adds higher than the nitric acid of cBN 2-3cm and boil 20 minutes, adds hydrochloric acid to boil 20 minutes after outwelling nitric acid, is washed till neutrality with distilled water.
4. the preparation method of strengthening polycrystalline cubic boron nitride composite superhard material as claimed in claim 1, is characterized in that, packs into strengthen stem stem body step and make to strengthen stem stem body and have more than 70% surface-area in mixing under powder parcel.
5. the preparation method of strengthening polycrystalline cubic boron nitride composite superhard material as claimed in claim 1, is characterized in that, the vacuum sphere time consuming of caking agent is greater than 24h.
6. the preparation method of strengthening polycrystalline cubic boron nitride composite superhard material as claimed in claim 1, is characterized in that, the time of vacuum reducing is greater than 24h.
7. the preparation method of strengthening polycrystalline cubic boron nitride composite superhard material as claimed in claim 1, is characterized in that, aftertreatment is pickling after pickling or ball milling.
8. the preparation method of the strengthening polycrystalline cubic boron nitride composite superhard material as described in claim 1-7 arbitrary, is characterized in that, the cross section of described enhancing stem stem body is circular, square or trilateral.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500778A (en) * | 2017-09-20 | 2017-12-22 | 陕西理工大学 | The preparation method of three kinds of dimension material coordination plasticizing polycrystalline cubic boron nitrides |
| CN111394633A (en) * | 2020-04-13 | 2020-07-10 | 富耐克超硬材料股份有限公司 | Superhard material polycrystalline compact |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103158287A (en) * | 2011-12-09 | 2013-06-19 | 郑州博特硬质材料有限公司 | Glomerocryst cubic boron nitride composite sheet and preparation method for same |
-
2014
- 2014-01-21 CN CN201410025088.2A patent/CN103755317B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103158287A (en) * | 2011-12-09 | 2013-06-19 | 郑州博特硬质材料有限公司 | Glomerocryst cubic boron nitride composite sheet and preparation method for same |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500778A (en) * | 2017-09-20 | 2017-12-22 | 陕西理工大学 | The preparation method of three kinds of dimension material coordination plasticizing polycrystalline cubic boron nitrides |
| CN111394633A (en) * | 2020-04-13 | 2020-07-10 | 富耐克超硬材料股份有限公司 | Superhard material polycrystalline compact |
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