阅读说明：本技术 一种高温高压培育彩色金刚石的方法 (A kind of method that high temperature and pressure cultivates fancy color diamond ) 是由 刘乾坤 易良成 赵鹏 申幸卫 卢洋 屈明 于 2019-08-08 设计创作，主要内容包括：本发明公开了一种高温高压培育彩色金刚石的方法,其中将高纯硼粉和高纯石墨按一定比例混合,并采用真空还原烧结,有效的保证了硼元素在碳源中的均匀分布和降低了碳源中有害杂质的含量。从而使蓝色培育钻石的颜色均匀性和产品内部净度都有很大提升。采用二次合成和辐照处理引入空位缺陷的工艺方法,根据绿色、红色、橙色、粉色、紫色金刚石的致色色心的差异,在二次合成时控制合成压力、合成温度和合成时间三个关键参数,可获得不同颜色的彩色金刚石。本发明工艺路线明确,合成方法简单、简便,结构稳定,可重复性强,有效实现了不同颜色的彩色金刚石的规模化生产,值得广泛推广应用。(The invention discloses a kind of methods that high temperature and pressure cultivates fancy color diamond, wherein high purity boron powder and high purity graphite are mixed in a certain ratio, and be sintered using vacuum reduction, boron element being uniformly distributed in carbon source is effectively guaranteed and reduces the content of objectionable impurities in carbon source.There is very big promotion to make blue cultivate the color homogeneity of diamond and interiors of products cleanliness.The process of vacancy defect is introduced using secondary synthesis and radiation treatment, according to the difference of green, red, orange, pink colour, purple diamond coloring colour center, three synthesis pressure, synthesis temperature and generated time key parameters are controlled in secondary synthesis, can get the fancy color diamond of different colours.Present invention process route is clear, and synthetic method is simple, easy, and stable structure, repeatability is strong, effectively realizes the large-scale production of the fancy color diamond of different colours, should be widely promoted application.)

1. a kind of method that high temperature and pressure cultivates fancy color diamond, which comprises the steps of:

(1) prefabricated synthesis stem, synthesis stem includes FeNi catalyst layer and carbon source layer, the two height ratio 1:1.0 ~ 1.5, FeNi The mass fraction of Ni is 65%-70% in catalyst layer, and it is of low quality in 0.3% high purity boron powder that the addition of carbon source layer accounts for carbon source, remaining at It is divided into high purity graphite, carbon source layer is after 1100 ~ 1200 DEG C of vacuum reductions are handled 20 ~ 24 hours, by synthesis stem and Synthetic block It assembles to obtain assembling block；

(2) assembling block is baked into 10-15h in 220 ~ 280 DEG C of baking ovens；

(3) the assembling block after the completion of baking, which is put into cubic hinge press, carries out the synthesis of first time high temperature and pressure, synthesis pressure 6- 6.5GP, synthesis temperature are 1250-1300 DEG C, and generated time is 5-7 days；

(4) synthesize after take out sample, using acid processing purification to get；

Or secondary high-temperature high-pressure synthesis will be carried out after the sample progress radiation treatment after acid processing purification, after secondary synthesis Take out sample, through peracid treatment purify to get.

2. the method that high temperature and pressure cultivates fancy color diamond according to claim 1, which is characterized in that the secondary high-temperature is high When being pressed into, the time is 5-10 hours, and synthesis temperature is 800-1500 DEG C, and synthesis pressure is in 5.5-6GP.

3. the method that high temperature and pressure cultivates fancy color diamond according to claim 1, which comprises the steps of:

When diamond obtained is blue diamond, process is as follows:

(1) prefabricated synthesis stem, synthesis stem includes FeNi catalyst layer and carbon source layer, the two height ratio 1:1.3, FeNi catalyst The mass fraction of Ni is 65%-70% in layer, and carbon source layer adds the high purity boron powder for accounting for carbon source quality 0.1%-0.3%, remaining ingredient is High purity graphite, carbon source layer assemble synthesis stem and Synthetic block after 1100 ~ 1200 DEG C of vacuum reductions are handled 20 ~ 24 hours Assembling block is obtained well；

(2) assembling block is baked into 10-15h in 220 ~ 280 DEG C of baking ovens；

(3) the assembling block after the completion of baking, which is put into cubic hinge press, carries out high temperature and pressure synthesis, synthesis pressure 6-6.5GP, Synthesis temperature is 1250-1300 DEG C, and generated time is 5-7 days；

(4) sample is taken out after synthesizing, using acid processing purification, just obtains required blue diamond.

4. the method that high temperature and pressure cultivates fancy color diamond according to claim 1, which comprises the steps of:

When diamond obtained is green, yellow, red or purple diamond, process is as follows:

(1) prefabricated synthesis stem, synthesis stem includes FeNi catalyst layer and carbon source layer, the two height ratio 1:1.3, FeNi catalyst The mass fraction of Ni is 65%-70% in layer, and carbon source layer is high purity graphite, and carbon source layer is by 1100 ~ 1200 DEG C of vacuum reduction processing After 20 ~ 24 hours, synthesis stem and Synthetic block are assembled to obtain assembling block；

(2) assembling block is baked into 10-15h in 220 ~ 280 DEG C of baking ovens；

(3) the assembling block after the completion of baking, which is put into cubic hinge press, carries out high temperature and pressure synthesis, synthesis pressure 6-6.5GP, Synthesis temperature is 1250-1300 DEG C, and generated time is 5-7 days；

(4) Synthetic block is taken out after synthesizing, using acid processing purification, Ib type is obtained and cultivates diamond；

(5) the Ib type of above-mentioned acquisition is cultivated into diamond and carries out radiation treatment, obtain green diamond；

(6) by containing the cultivation diamond after radiation treatment with high purity graphite powder by Volume fraction 1:(5 ~ 7) mix and be pressed into Stem is synthesized, synthesis stem and Synthetic block assemble to obtain assembling block；

(7) assembling block is baked into 10-15h in 220 ~ 280 DEG C of baking ovens；

(8) the assembling block after the completion of baking, which is put into cubic hinge press, carries out high temperature and pressure secondary synthesis, generated time 5-10 Hour, synthesis temperature is within the scope of 800-1500 DEG C, and synthesis pressure is in 5.5-6GP；

(9) sample is taken out after synthesizing, using acid processing purification, just obtains red or purple diamond.

5. the method that high temperature and pressure cultivates fancy color diamond according to claim 3, which is characterized in that irradiation in step (5) Handling the time is 3-5 hours, and irradiation dose is about 40-100MGy.

6. the method that according to claim 1 or 3 or 4 high temperature and pressure cultivate fancy color diamond, which is characterized in that high purity boron powder Purity >=99.99%, purity >=99.9999% of high purity graphite.

Technical field

The invention belongs to superhard materials to be synthetically produced technical field, and in particular to a kind of high temperature and pressure cultivation fancy color diamond Method.

Background technique

Diamond is in the diamond after manual polishing, currently, the diamond of discovery has colourless, yellow, green, red, orange Color, blue, pink colour, purple, black etc., the color of diamond are almost covered from purple to red entire spectrum colour system.According to For now more perfect diamond coloring is theoretical, different colours are presented in diamond, are primarily due to defect different inside diamond Caused, different defects and defect combination makes diamond that different colours be presented.More well-known diamond color formation theory Have: band theory, defect colour system coloring, plastic deformation coloring, inclusion enclave coloring etc..

HPHT(high pressure-temperature) synthetic method be imitate natural diamond growing environment, grown in the environment of manually providing A kind of method of diamond out.ASEA company, Switzerland has synthesized artificial diamond in nineteen fifty-three at first, and subsequent AM General is public It takes charge of and also announced to have synthesized artificial diamond in 1954.Cubic hinge press is China's independent research, has perfect knowledge property right High temperature and pressure synthesis device, have become the main equipment of whole world artificially synthesizing diamond at present.This technology be exactly It is different according to the color-causing mechanism of different colours diamond on domestic cubic hinge press, in high temperature and pressure synthesis process, pass through introducing Color-causing element or artificial manufacture diamond internal flaw, to obtain the artificial culture fancy color diamond of different colours.

Summary of the invention

The present invention is different according to the color-causing mechanism of different colours diamond based on temperature differential method, synthesizes in high temperature and pressure In the process, by being artificially introduced color-causing element or manufacture diamond internal flaw, to obtain the artificial culture gold of different colours Hard rock.This synthetic process is simple and reliable, works well, and has been greatly improved the output capacity of fancy color diamond, realizes artificial Cultivate the large-scale production of fancy color diamond.The technical solution adopted in the present invention, according to the Buddha's warrior attendant for the different colours of being obtained Stone product has formulated different processing technology routines.

A kind of method that high temperature and pressure cultivates fancy color diamond, includes the following steps:

(1) prefabricated synthesis stem, synthesis stem includes FeNi catalyst layer and carbon source layer, the two height ratio 1:1.0 ~ 1.5, FeNi The mass fraction of Ni is 65%-70% in catalyst layer, and it is of low quality in 0.3% high purity boron powder that the addition of carbon source layer accounts for carbon source, remaining at It is divided into high purity graphite, carbon source layer will synthesize stem after 1Pa or less, 1100 ~ 1200 DEG C of vacuum reductions are handled 20 ~ 24 hours It assembles to obtain assembling block with Synthetic block；

(2) assembling block is baked into 10-15h in 220 ~ 280 DEG C of baking ovens；

(3) the assembling block after the completion of baking, which is put into cubic hinge press, carries out the synthesis of first time high temperature and pressure, synthesis pressure 6- 6.5GP, synthesis temperature are 1250-1300 DEG C, and generated time is 5-7 days；

(4) synthesize after take out sample, using acid processing purification to get；

Or secondary high-temperature high-pressure synthesis will be carried out after the sample progress radiation treatment after acid processing purification, after secondary synthesis Take out sample, through peracid treatment purify to get.

Further, include the following steps:

When diamond obtained is blue diamond, process is as follows:

(1) prefabricated synthesis stem, synthesis stem includes FeNi catalyst layer and carbon source layer, the two height ratio 1:1.3, FeNi catalyst The mass fraction of Ni is 65%-70% in layer, and carbon source layer adds the high purity boron powder for accounting for carbon source quality 0.1%-0.3%, remaining ingredient is High purity graphite, carbon source layer is after 1Pa or less, 1100 ~ 1200 DEG C of vacuum reductions are handled 20 ~ 24 hours, by synthesis stem and conjunction It is blocking to assemble to obtain assembling block；

(2) assembling block is baked into 10-15h in 220 ~ 280 DEG C of baking ovens；

(3) the assembling block after the completion of baking, which is put into cubic hinge press, carries out high temperature and pressure synthesis, synthesis pressure 6-6.5GP, Synthesis temperature is 1250-1300 DEG C, and generated time is 5-7 days；

(4) sample is taken out after synthesizing, using acid processing purification, just obtains required blue diamond.

Further, include the following steps:

When diamond obtained is green, yellow, red or purple diamond, process is as follows:

(1) prefabricated synthesis stem, synthesis stem includes FeNi catalyst layer and carbon source layer, the two height ratio 1:1.3, FeNi catalyst The mass fraction of Ni is 65%-70% in layer, and carbon source layer is high purity graphite, and carbon source layer passes through 1Pa or less, 1100 ~ 1200 DEG C of vacuum After reduction treatment 20 ~ 24 hours, synthesis stem and Synthetic block are assembled to obtain assembling block；

(2) assembling block is baked into 10-15h in 220 ~ 280 DEG C of baking ovens；

(3) the assembling block after the completion of baking, which is put into cubic hinge press, carries out high temperature and pressure synthesis, synthesis pressure 6-6.5GP, Synthesis temperature is 1250-1300 DEG C, and generated time is 5-7 days；

(4) Synthetic block is taken out after synthesizing, using acid processing purification, Ib type is obtained and cultivates diamond；

(5) the Ib type of above-mentioned acquisition is cultivated into diamond and carries out radiation treatment, obtain green diamond；

(6) by containing the cultivation diamond after radiation treatment with high purity graphite powder by Volume fraction 1:(5 ~ 7) mix and be pressed into Stem is synthesized, synthesis stem and Synthetic block assemble to obtain assembling block；

(7) assembling block is baked into 10-15h in 220 ~ 280 DEG C of baking ovens,；

(8) the assembling block after the completion of baking, which is put into cubic hinge press, carries out high temperature and pressure secondary synthesis, generated time 5-10 Hour, synthesis temperature is within the scope of 800-1500 DEG C, and synthesis pressure is in 5.5-6GP；

(9) sample is taken out after synthesizing, using acid processing purification, just obtains red or purple diamond.

Further, the radiation treatment time is 3-5 hours in step (5), and irradiation dose is about 40-100MGy.

Purity >=99.99% of high purity boron powder, purity >=99.9999% of high purity graphite.

The beneficial effects of the present invention are:

The present invention is different according to the color-causing mechanism of different colours diamond, in high temperature and pressure synthesis process, by being artificially introduced Impurity element or manufacture diamond internal flaw, to obtain the artificial culture diamond of different colours.Synthesis assembling block is set During meter, the common temperature differential method package assembly of diamond is cultivated using Gem Grade.

During synthesis blue cultivates diamond, high purity boron powder and high purity graphite are mixed in a certain ratio, and using true Sky reduction sintering, is effectively guaranteed boron element being uniformly distributed in carbon source and reduces the content of objectionable impurities in carbon source. There is very big promotion to make blue cultivate the color homogeneity of diamond and interiors of products cleanliness.

When carrying out green, red, yellow, purple diamond artificial culture, using the process of secondary synthesis, first make At diamond semi-finished product, vacancy defect is artificially introduced inside diamond by radiation treatment, further according to green, yellow, red, The difference of the coloring colour center of purple diamond controls synthesis pressure, synthesis temperature and generated time three passes in secondary synthesis Bond parameter obtains the fancy color diamond of different colours.

Using FeNi as catalyst material in the present invention, wherein the mass fraction of Ni is 65%-70%, and carbon is effectively guaranteed Solubility and migration velocity of the element in catalyst layer mention to greatest extent while guaranteeing to cultivate cleanliness inside diamond The high speed of growth of diamond crystal, effectively shortens generated time.

Present invention process route is clear, and synthetic method is simple, easy, and stable structure, repeatability is strong, effectively realizes not With the large-scale production of the fancy color diamond of color, should be widely promoted application.

Detailed description of the invention

Fig. 1 is that the assembling block and embodiment 2 when embodiment 1 synthesizes blue diamond after assembling synthesize green, red Buddha's warrior attendant Assembling block when first time high temperature and pressure synthesizes when stone after assembling, 1. pyrophyllite in lumps in figure, 2. conductive plugs, 3. pyrophillite rings, 4. dolomite outer lining, 5. carbon paper pipes, 6. carbon paper pieces, 7. magnesia liners, 8. carbon source layers, 9.FeNi catalyst layer, 10. brilliant beds；

Assembling block when Fig. 2 is second of high temperature and pressure synthesis when embodiment 2 synthesizes green, red diamond after assembling, in figure 1. pyrophyllite in lumps, 2. conductive plugs, 3. pyrophillite rings, 4. dolomite outer linings, 5. carbon paper pipes, 6. carbon paper pieces, in 7. magnesia Lining, 11. graphite stems, 12. diamond semi-finished product；

Fig. 3 is the blue diamond product that embodiment 1 obtains；

Fig. 4 is the Ib type diamond (figure a) that a high temperature and pressure synthesizes in embodiment 2, and irradiated processing becomes green (figure B), in the procedure chart for becoming red (figure c) by secondary synthesis processing；

Fig. 5 is embodiment 2 under other conditions same case, keeps production obtained by 1h and 800 DEG C of holdings 1h for 700 DEG C when secondary synthesis The infrared spectrogram of product.

Specific embodiment

Below in conjunction with drawings and examples, further details of the technical solution of the present invention, but not as to this hair The limitation of bright protection scope.